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Journal articles on the topic 'Pharmacy Chromatographic analysis'
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Sharmin, Suriya, Md Hossain Sohrab, Fatema Moni, Farhana Afroz, Satyajit Roy Rony, and Shammi Akhter. "Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets." Pharmacia 67, no. 4 (November 27, 2020): 383–91. http://dx.doi.org/10.3897/pharmacia.67.e57981.
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A reverse phase liquid chromatographic method for estimation of Aceclofenac in bulk drug and tablet dosage form was developed and validated. The chromatographic conditions to achieve the highest performance parameters using octylsilyl column with guard filter were optimized. The separation was carried out using a mobile phase containing 10 mM Phosphate Buffer, pH 2.1 and methanol (30:70% v/v) pumped at a flow rate of 1.0 mL/min with detection at 272 nm. The method was shown to be linear in 19.8–148.5 μg/mL concentration range (regression coefficient of 0.999). The limit of detection (LOD) and limit of quantification (LOQ) was found to be 0.0692 μg/mL and 0.2076 μg/mL, respectively. The accuracy of the method was assessed by adding fixed amount of pre-analyzed sample to different standard solutions (80%, 100%, and 120% of the tested concentration) in triplicate. The percentage mean recoveries were 97.91% to 100.39% with %RSD values of 0.64–0.79. The method was found to be precise with %RSD value of 1.13 and 1.60 for intraday and interday precision study, respectively. The method specificity and robustness were also established. New and sensitive HPLC method for estimation of Aceclofenac has been developed, in respect to the reviewed analytical methods.
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Savic, Ivan, Goran Nikolic, Ivana Savic, and Milorad Cakic. "The application of HP-GFC chromatographic method for the analysis of oligosaccharides in bioactive complexes." Chemical Industry 63, no. 5 (2009): 415–26. http://dx.doi.org/10.2298/hemind0905415s.
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The aim of this work was to optimize a GFC method for the analysis of bioactive metal (Cu, Co and Fe) complexes with olygosaccharides (dextran and pullulan). Bioactive metal complexes with olygosaccharides were synthesized by original procedure. GFC was used to study the molecular weight distribution, polymerization degree of oligosaccharides and bioactive metal complexes. The metal bounding in complexes depends on the ligand polymerization degree and the presence of OH groups in coordinative sphere of the central metal ion. The interaction between oligosaccharide and metal ions are very important in veterinary medicine, agriculture, pharmacy and medicine.
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Golembiovska, Оlena, Oleksii Voskoboinik, Galina Berest, Sergiy Kovalenko, and Liliya Logoyda. "Quality by design approach for simultaneous determination of original active pharmaceutical ingredient quinabut and its impurities by using HPLC. Message 1." Pharmacia 68, no. 1 (January 7, 2021): 79–87. http://dx.doi.org/10.3897/pharmacia.68.e50704.
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Aim. The aim of study was to develop and validate a simple, highly robust (quality by design (QbD) approach), precise and accurate method using high performance liquid chromatography for the simultaneous determination of original active pharmaceutical ingredient Quinabut and its impurities. Materials and methods. Experiments were performed on a Shimadzu LC-20 Prominence HPLC separation module, equipped with a quaternary gradient pump, temperature controlled column heater, sampler manager and diode array detector and LC-20 Chemstation for data analysis (Shimadzu Corporation, Japan). Same software was used for data acquisition and processing of results. X-Terra RP18 (4.6×150 mm, 5 μm) analytical chromatographic column provided by Waters Corporation (Milford, MA) was used for all optimization experiments. Mobile phase A: acetonitrile R. Mobile phase B: 0.025 M phosphate buffer solution. Samples were chromatographed in gradient mode. Flow rate of the mobile phase: 0.7 mL/min. Column temperature: 40 °С. Detection: at 233 nm wavelength. Injection volume: 50 μl. Results. Screening of the influence of four chromatographic factors on different chromatographic responses was performed as the initial step of analytical method optimization. A randomized fractional factorial experimental design (24–1) of resolution IV with central point was used. Buffer pH, amount of acetonitrile in mobile phase A, the amount of phosphate buffer solution in mobile phase B and column temperature were selected as factors of interest, and were used to generate the fractional factorial experimental design. Linearity was established in the range of LOQ level to 0.2% having regression coefficients 0.9977. Calibration curve – y = 0.0132 + 0.9902. Since Δt for the content of quinabut is less than max δ, the technique is stable over time. The possibility of contamination of the sample by decomposition products by keeping it under stressful conditions (irradiation of the substance solution with UV light (UV irradiation with mercury lamp light); acid hydrolysis with 0.1 M hydrochloric acid solution; oxidative decomposition) was investigated. As a result of the irradiation with UV light, the impurity peaks for about 8.74 min (impurity C) and 12.68 min (impurity B) are additionally revealed. Their content exceeds the limits of normalization and is 0.6% and 3.7%, respectively. Therefore, the powder of the substance and its solutions should be stored away from direct sunlight. The column temperature and the speed of the mobile phase within ± 10% did not significantly affect the test results. The results were found to be within the assay variability limits during the entire process. Conclusion. 1) The optimization of a new analytical method capable of simultaneous determination of quinabut assay and its impurities drug products was performed with a single fractional factorial experimental design. Only 11 experiments were needed for the optimization, while at least 16 experiments would be needed to cover the same analytical method operational region of the first optimization step with a traditional one factor at time (OFAT) approach. 2) HPLC method was developed and validated for the simultaneous detection and quantitation of quinabut and its impurities. 3) The final analytical method optimized with QbD approach was validated according to ICHQ2R1 guideline. The method proved to be sensitive, selective, precise, linear, accurate and stability-indicating. 4) The method was successfully applied to the analysis of demonstrating acceptable precision and adequate sensitivity for the detection and quantitation of quinabut and its impurities. So it may be reasonable to claim that the method can be extended to the analysis of drug formulations and stability samples as well. This optimization reflects in saving of time and resources since one stability study includes hundreds of samples tested during the product’s shelf life.
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Synbulatov, IV V., A. V. Voronin, and T. V. Voronina. "ANALYsis oF RYRRoLIDiNopHENoNE DERivATivEs iN BioLoGiOAL FLuiDs." Aspirantskiy Vestnik Povolzhiya 19, no. 1-2 (March 15, 2019): 33–40. http://dx.doi.org/10.17816/2072-2354.2019.19.1.33-40.
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Pyrrolidinophenone derivatives are the group of narcotic drugs controlled in the Russian Federation. The review presents the trends of biotransformation of а-pyrrolidinovalerophenone and 3,4-methylenedioxypyrovalerone, the data about their primary metabolites is provided. Various techniques of the sample preparation of biological fluids for analytical toxicology studies for substances of the pyrrolidinophenone derivative group are discussed. The use of enzymatic hydrolysis followed by solid-phase extraction (sorption) provides low detection limits for native sub- PHARMACY ФАРМАЦИЯ stances of this group and primary metabolites using small volumes of biological fluids (0.5 and 1.0 ng/ml blood for a-pyrrolidinovalerophenone and 3,4-methylenedioxypirovalonone respectively). The main characteristics of pyrro-lidinophenone derivatives (Kovac’s retention indices in nonpolar stationary liquid phases and the main characteristic ions in the mass spectra of electron impact) are presented. They allow to identify pyrrolidinophenone derivatives and their primary metabolites in biological fluids during chromatographic-mass spectrometric screening. Analytical possibilities of an alternative variant of screening for biological fluids i.e. analysis by using current immunochemical test systems, including “biochips” are discussed. The main methods of reliable identification and quantitative determination of pyrrolidinophenone derivatives are chromatography-mass spectrometry and high-performance liquid chromatography-tandem mass spectrometry. The detection limit of 3,4-methylenedioxypyralovalone in blood by gas chromatography-mass spectrometry is 1.0 ng/ml. The ranges of the determined concentrations of the method of quantitation by gas chromatography-mass spectrometry are 2.0-2000.0 ng/ml for blood and 0.05-50.0 ng/10 mm for hair. The high-performance chromatography-tandem mass spectrometry method with a triple quadrupole in the monitoring mode of multiple molecular reactions makes it possible to achieve a nearly complete suppression of analytical background “noise” for a sample, and to obtain detection and quantification limits for 3,4-methylenedioxypy-raloperone in cadaveric blood at a level of 10.0-100.0 pg/ml and 1.0-10.0 ng/ml, respectively. One of the advantages of the high-performance chromatography-tandem mass spectrometry system is the screening possibility.
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ROCHA, Juliana Almeida, Vanessa de Andrade ROYO, and Elytania Veiga MENEZES. "BIODIESEL PRODUCTION AND PAPER CHROMATOGRAPHY IN ORGANIC CHEMISTRY TEACHING." Periódico Tchê Química 13, no. 26 (August 20, 2016): 52–58. http://dx.doi.org/10.52571/ptq.v13.n26.2016.52_periodico26_pgs_52_58.pdf.
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Biodiesel is important renewable energy that stands out mainly due to the possible reduction of oil reserves and environmental impacts intensified by the use of fossil fuels. This biofuel is produced from various oily materials, catalysts, and alcohols. Generates glycerin as a byproduct, which is used in different kinds of industries. Given the importance of the fuel and the need to integrate the theoretical content with the practical application of knowledge, this article aims to describe an experiment that can be used for teaching content such as chromatography and transesterification reaction in graduation courses. For biodiesel production were used: soybean oil, methanol, and potassium hydroxide, and analysis on paper chromatography were employed: filter paper and the solvents hexane, ethyl ether, and acetic acid as eluants. The viscosity and specific gravity of soybean oil and biodiesel were measured. With experiments, the academics observed that the transesterification reaction changes the physical-chemical properties of oil when it is converted into biodiesel and understand basic principles governing the chromatographic techniques and organic reactions.
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PRAZERES, Raissa Mendes, Kamylla Teixeira SANTOS, Afrânio Farias de MELO JUNIOR, Dario Alves de OLIVEIRA, Elytânia Veiga MENEZES, José Bento SAMPAIO-JÚNIO, Francine Souza Alves FONSECA, and Vanessa de Andrade ROYO. "FATTY ACID PROFILE AND PHYSICAL CHEMICAL PROPERTIES OF OIL EXTRACTED FROM Banisteriopsis pubipetala (A.Juss.) Cuatrec. (MALPIGHIACEAE) SEEDS." Periódico Tchê Química 14, no. 27 (January 20, 2017): 105–11. http://dx.doi.org/10.52571/ptq.v14.n27.2017.105_periodico27_pgs_105_111.pdf.
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The species Banisteriopsis pubipetala (Malpighiaceae), occurs in the Brazilian cerrado, is a liana has anemochorous fruits with small seeds and lipid reserves. There are few studies on this species and the importance of investigating the composition occurs, due to other species of the same genus be studied and they have diverse biological activities. This study aimed to evaluate the presence of volatile compounds in the seeds by Headspace, fatty profile by gas chromatography coupled to mass spectrometry and the physicochemical properties of the oil extracted from the seeds of Banisteriopsis pubipetala. From the chromatographic analysis fatty acids were identified: palmitic, oleic, linoleic and eicosanoic. It has been found absence of volatile compounds in seeds. The physicochemical properties evaluated were: seed oil content (41%), moisture content (4.2%), pH (5.25), ash (0.08% m/m), acidity index (1.0 mg KOH·g-1), iodine (cg I2·g-1) and peroxides (0.5 meq·kg-1). The results were similar to other species of the same family and the cerrado. This information is the foundation for developing future research, since it is relevant to assess the possibility of bioprospecting and possible industrial use of this input, for example, in the pharmaceutical and cosmetic industry because of fatty acids present.
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Павлюк, Б. В., Ю. Я. Мельник, Т. А. Грошовий, М. Б. Чубка, and В. Й. Скорохода. "Research of water extraction from xenoderm as an active pharmaceutical ingredient in drugs." Farmatsevtychnyi zhurnal, no. 5 (October 1, 2020): 42–50. http://dx.doi.org/10.32352/0367-3057.5.20.05.
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Today, burns are one of the most common types of injuries in the home and at work around the world. Therefore, the issue of treatment of burns remains relevant today for medicine and pharmacy in particular.
In Ukraine, the method of treatment of burns using xenodermoimplants from porcine skin is used, and therefore the crushed substrate of cryolyophilized porcine skin (xenoderm) is a promising active ingredient in the technology of various drug forms.
The aim of the work was to study the structural and mechanical properties of water extract from the crushed substrate of the xenoderm and to determine its amino acid composition by using physicochemical analysis, namely using high performance liquid chromatography (HPLC).
A glass pycnometer and a Heppler BH 2 MLW drop ball viscometer were used to determine the density and viscosity of the water extract from the xenoderm. The density and viscosity of the water extract were studied at different temperatures.
The dependence of the density and viscosity of the water extract from the xenoderm on temperature was studied and it was found that with increasing temperature the dynamic viscosity decreases and the density changes slightly.
A glass pycnometer and a viscometer with falling ball were used to determine the density and viscosity of the xenoderm water extract. Chromatographic separation of amino acids was performed on a liquid chromatograph Agilent 1200 with a fluorescent detector.
Chromatographic determination of amino acids was performed on a liquid chromatograph Agilent 1200 (USA) with a fluorescent detector G1315A (USA) and an autosampler 1313A.
Using the HPLC method, 16 amino acids were identified (essential – 6; conditionally – 2; nonessential – 8). Identified amino acids are almost in a bound state (1.5%), the largest amount is glutamic acid (0.23%), glycine (0.19%), aspartic acid (0.18%), proline (0.17%) and arginine (0.17%). In unbound form, the content of glutamic acid (0.09%) and glycine (0.06%) is the highest.
Based on the results of research, you can choose quality indicators, to determine the appropriate criteria that can be proposed for the standardization of water extract from the crushed substrate of the xenoderm.
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Golembiovska, Оlena, Oleksii Voskoboinik, Galina Berest, Sergiy Kovalenko, and Liliya Logoyda. "Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2." Pharmacia 68, no. 1 (January 7, 2021): 53–59. http://dx.doi.org/10.3897/pharmacia.68.e52119.
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Aim. The aim of study was to develop and validate a simple, precise and accurate method using gas chromatography for analysis of residual solvents – acetone and 2-propanol – in quinabut API. Materials and methods. All experiments were performed on a gas chromatographic system equipped with FID detector (Shimadzu GC System) using the DB-624 (30 m × 0.32 mm ID, 3.0 μm film sickness) column as stationary phase. Nitrogen was used as carrier gas with flow rate 7.5 mL/ min. Split ratio was 1:5, injector temperature was 140 °C, detector temperature was 250 °C, oven temperature was programmed from 40 °C (2 min) to 50 °C at 1 °C/min and then increased at a rate of 15 °C/min up to 215 °C; and maintained for 2 min. All solutions were prepared using water as diluent. Results. This proposed method is assessed for separation of residual solvent from quinabut with quantification. The obtained results are compared with the corresponding specified limits of ICH standard guidelines. The method validation was done by evaluating specificity, limit of detection (LOD) and limit of quantitation (LOQ), linearity, accuracy, repeatability, ruggedness, system suitability and method precision of residual solvents as indicated in the ICH harmonized tripartite guideline. The separation between acetone and 2-propanol peaks is 2.07. Hence method was found to be specific. The linear relationship evaluated across range of 15 to 180% for acetone and 2-propanol of ICH specified limit of residual solvents. The graphs of theoretical concentration versus obtained concentration are linear and the regression coefficients ‘R’ for residual solvents were more than 0.9968. The values of LOD and LOQ were much less than the lower limit of the concentration range and cannot affect the accuracy of the test. The technique was characterized by high intra-laboratory accuracy at concentrations close to the nominal acetone and 2-propanol concentration. All solutions were stable in water for at least 1 hour when stored at room temperature. Conclusion. A simple, specific, accurate, precise and rugged gas chromatography method was developed and validated for the quantification of residual solvents present in quinabut API through an understanding of the synthetic process, nature of solvents and nature of stationary phases of columns. The residual solvents acetone and 2-propanol were determined.
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Peleshok, K. Ye, L. S. Logoyda, and O. B. Poliak. "DEVELOPMENT AND METHODOLOGY FOR THE ESTIMATION OF ATENOLOL AND VALSARTAN IN PHARMACEUTICALS." Здобутки клінічної і експериментальної медицини, no. 1 (May 5, 2020): 30–33. http://dx.doi.org/10.11603/1811-2471.2020.v.i1.11066.
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According to the appropriate protocols for the treatment of hypertension are often used antihypertensive drugs of the 5 main classes – first-line drugs, which when used in equivalent doses contribute to the reduction of blood pressure and significantly reduce the risk of cardiovascular complications. Quite often, doctors prescribe two/three medicines at a time. Therefore, the creation of fixed combinations antihypertensive action in the form of solid dosage forms is an urgent task of modern pharmacy.
The aim of the study – to improve to more rapid, simple, selective, less expensive methods TLC analysis of simultaneous determination of atenolol and valsartan in pharmaceuticals.
Methods. The present study assessed mobile phases of atenolol and valsartan for TLC.
Results and Discussion. Method of simultaneous identification of atenolol and valsartan by TLC has been developed. We have established that the most optimal Rf observed using mobile phases for simultaneous determination of atenolol and valsartan: n-butanol-acetic acid-water (40:10:20). We have explored the validation characteristics – specificity and suitability of the chromatographic system that met, the eligibility criteria established by the SPU.
Conclusion. We have developed chromatographic method for simultaneous determination of atenolol and valsartan. Prospects for future research will be aimed at developing analytical methods of analysis.
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Vree, T. B., A. M. Baars, and E. W. Wuis. "Direct high pressure liquid chromatographic analysis and preliminary pharmacokinetics of enantiomers of oxazepam and temazepam with their corresponding glucuronide conjugates." Pharmaceutisch Weekblad Scientific Edition 13, no. 2 (April 1991): 83–90. http://dx.doi.org/10.1007/bf01974986.
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Kyslychenko, O. A., Viktoriia V. Protska, and Iryna O. Zhuravel. "HPLC determination of phenolic compounds content in Parmelia sulcata and Parmelia vagans thalli." Pharmacia 66, no. 4 (December 31, 2019): 161–64. http://dx.doi.org/10.3897/pharmacia.66.e35194.
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The species of Parmelia genus have long been used in Indian folk medicine for the treatment of bronchitis, ulcers, furunculosis, cardiovascular diseases, urolithiasis, amenorrhea, and also at infectious and inflammatory diseases. In Ukraine, the most common lichens of the Parmelia genus are Parmelia sulcata Tailor and Parmelia vagans Nyl. At the same time, thalli of Parmelia genus lichens belong to the non-officinal and poorly studied types of raw material. The qualitative composition and the quantitative content of phenolic compounds in Parmelia sulcata and Parmelia vagans thalli was studied by HPLC. According to the results of the chromatographic analysis, salazinic, fumaroprotocetraric, usnic acids, chloratranorin and atranorin were identified in both types of raw material studied. In addition, protocetraric acid was identified in Parmelia sulcata thalli. According to the results of the experiment, the total content of identified phenolic compounds in Parmelia sulcata thalli was 2019.71±40.39 g/mol, and in Parmelia vagans thalli it comprised 1754.18±34.77 g/mol. In the thalli of both studied species of Parmelia genus, fumaroprotocetraric acid dominanted by the quantity. This substance was present in Parmelia sulcata thalli in the amount of 474.00±9.00 g/mol, and in Parmelia vagans thalli – 456.21±8.67 g/mol. In addition, a significant amount of chloratranorin (408.79±8.99 g/mol) was present in Parmelia sulcata thalli. Quite a high content of atranorin (393.34±8.65 g/mol) and usnic acid (375.31±7.53 g/mol) were defined in Parmelia vagans thalli. The results obtained can be used in the development of quality control methods for Parmelia sulcata and Parmelia vagans thalli, as well as medicines based on these types of raw materials.
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Wilson, Phyllis. "Development and Validation of a Liquid Chromatographic Method for the Simultaneous Determination of Estradiol, Estriol, Estrone, and Progesterone in Pharmaceutical Preparations." Journal of AOAC INTERNATIONAL 92, no. 3 (May 1, 2009): 846–54. http://dx.doi.org/10.1093/jaoac/92.3.846.
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Abstract Progesterone and estrogens are hormones produced in the human body that are essential for regulating many vital functions. The three major estrogens produced by women are estriol, estradiol, and estrone. Progesterone is a naturally occurring hormone in both men and women. Pharmaceuticals containing estrogens alone or estrogens in combination with progesterone are commonly used in therapy. Patients requiring unique combinations of the drugs rely on pharmacies to compound the ingredients. In order to assess the potency of drugs containing combinations of estrogens and progesterone, a method was developed to determine all four ingredients simultaneously. The liquid chromatographic method utilized a Bondapak C18 column with an isocratic mobile phase of acetonitrilewater (50 + 50, v/v) at a flow rate of 1.0 mL/min and temperature of 30C. Under these conditions, the order of elution was estriol, estradiol, and estrone, followed by progesterone. UV detection was at 205 nm to monitor elution of the estrogens, then switched to 270 nm to monitor progesterone. The method was applied to the analysis of pharmacy-compounded drugs containing combinations of the hormones. Validation studies demonstrated that the method is accurate and precise.
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Vree, T. B., E. W. J. Beneken Kolmer, and Y. A. Hekster. "High pressure liquid chromatographic analysis and preliminary pharmacokinetics of sulfaphenazole and its N2-glucuronide and N4-acetyl metabolites in plasma and urine of man." Pharmaceutisch Weekblad Scientific Edition 12, no. 6 (December 1990): 243–46. http://dx.doi.org/10.1007/bf01967825.
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Piponski, Marjan, Trajan Balkanov, and Liliya Logoyda. "Development and validation of a fast and simple HPLC method for the simultaneous determination of bisoprolol and enalapril in dosage form." Pharmacia 68, no. 1 (January 7, 2021): 69–77. http://dx.doi.org/10.3897/pharmacia.68.e50919.
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Aim. We aimed to develop and validate fast, simple, accurate, robust and rugged chromatographic method for simultaneous determination of bisoprolol fumarate and enalaril maleate in solid pharmaceutical dosage form, with using chaotropic strong chaotropic perchlorate anions in composition of mobile phase. Materials and methods. Fast simple HPLC method for simultaneous determination of bisoprolol and enalapril in solid pharmaceutical dosage forms was developed, with perfect peak symmetries eluting at 4.7 and 5.2 miutes, with mobile phase composed of methanol and diluted perchloric acid pumped with 1ml/min on Zorbax Rx C8 250x4.6mm, 5um column thermostated at 42 °C, and monitored UV signal at 214nm. Mobile phase was composed of 55%methanol and 45% perchloric acid (0.07%v/v). Results. Usage of presence of perchloric anions showed very useful role in peak shape and chromatogram view, due to distinguished chaotropic characteristics of perchlorate anions on molecules containing nitrogen atoms in molecular structures of analytes, in acidic pH environment. Linearity was examined and proven at different concentration levels in the range of working concentration of bisoprolol (20–200 ug/ml) and enalapril (20–200 ug/ml). The methods achieved very good validation parameters, with determined LOQ about 0.032 mg/ml and LOD about 0.003 mg/ml for bisoprolol, and LOQ about 0.045 mg/ml and LOD 0.005 mg/ml for enalapril. The high value of recoveries obtained for bisoprolol and enalapril indicates that the proposed method was found to be accurate. Conclusion. A new fast and simple, but selective, accurate, precise and robust HPLC method for simultaneous determination of bisoprolol and enalapril in tablets was developed and many possible variations of the same were suggested. The developed method for the simultaneous quantification of bisoprolol and enalapril from solid dosage formulations offers simplicity essential for quality control of a large number of samples in short time intervals, which is necessary for routine analysis.
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PINHEIRO, Helilma de Andréa, Ana Paula Mota FERREIRA, Ismael Carlos Braga ALVES, Antônio Fernandes SANTOS JÚNIOR, Raquel Bezerra dos Santos SAWCZUK, helmara diniz costa VIEGAS, Aldaléa Lopes Brandes MARQUES, and Gilvanda Silva NUNES. "DETERMINATION OF BTEX IN ENVIRONMENTAL SAMPLES: DEVELOPMENT AND PROTECTION OF TECHNOLOGIES AND ANALYTICAL METHODS." Periódico Tchê Química 16, no. 31 (January 20, 2019): 431–39. http://dx.doi.org/10.52571/ptq.v16.n31.2020.437_periodico31_pgs_431_439.pdf.
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The contamination of water and soil by petroleum hydrocarbons is reported quite frequently, mainly due to accidents involving transport and storage of fuels. Among the most toxic compounds the most volatile benzene, toluene, ethylbenzene and xylene (BTEX). Residues of these compounds can cause serious environmental and public health troubles. Thus, more sensitive, selective and low-cost techniques, focused on the analysis and monitoring of these contaminants are being developed in order to establish operational control and to comply with local laws, but the intellectual property of such technologies is still unknown. The present study shows the panorama about patents, thesis and dissertations which have been already published on this theme. Together, the United States and China hold the largest number of patents, and most of thesis/dissertations describe methodologies for BTEX detection in water, although numerous environmental problems caused by oils in the soil had been reported. Also, the methods based on chromatographic techniques stand out in relation to the other techniques. It was possible to verify important advances in the field of sensors, especially the electrochemical ones, in order to solve the analytical gaps.
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Peleshok, Kateryna, Marjan Piponski, Elizabeth Adaeze Ajie, Olha Poliak, Nadiya Zarivna, Olha Denefil, and Liliya Logoyda. "Novel HPLC-UV method for simultaneous determination of valsartan and atenolol in fixed dosage form; Study of green profile assessment." Pharmacia 68, no. 1 (January 7, 2021): 43–51. http://dx.doi.org/10.3897/pharmacia.68.e53631.
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Aim of this work was to develop the first simple, rapid, green, economical and selective HPLC method for simultaneous quantification of the cited drugs in their challenging binary mixture. The work was motivated by the global trends towards sustainable chemistry in designing eco-friendly mobile system without affecting the analysis parameters. The proposed method was subjected to a greenness profiles using some metrics as Eco-scale. Materials and methods. This was accomplished under the following chromatographic conditions: HPLC column Discovery C18 (4.6 mm i.d. × 150 mm, 5 μm), column temperature 30 °C, flow rate 1.0 mL/min, mobile phase composed of 20% acetonitrile, 80% of 0.16% ammonium acetate and 0.2% of 1.5 M tetramethylammonium hydroxide (V/V) and signal monitoring at a wavelength of 225 nm and 237 nm. Results. A conventional mixture of acetonitrile and 0.16% ammonium acetate was tried in different ratios, but the drugs were not well separated. The shortest aliphatic chain cationic ion pair reagent tetramethylammonium hydroxide should not be exchanged with other type similar with this, like tetramethylammonium hydrogen sulfate, it did not work to our experiments. Increasing salt concentration, ammonium acetate, more than 0.2%, pushes the peak of atenolol closer to dead volume, which is negative. Atenolol in their methods for multicomponent mixtures elutes in dead volume, or when retained longer, much stronger, hydrophobic mobile phase should be used if valsartan should be seen in same chromatogram at dissent time. The 237 nm can be chosen as compromise signal for nearly equal peaks height with high sensitivity is not essential. The 225 nm signal shows much higher sensitivity for atenolol and less increase for valsartan peaks, which can be used when higher sensitivities will be essential. Linearity was examined and proven at different concentration levels in the range of working concentration of valsartan (0.16–0.96 mg/mL) and atenolol (0.2–1.20 mg/mL). The high value of recoveries obtained for valsartan and atenolol indicates that the proposed method was found to be accurate. The results of proposed method found to be an excellent green analysis with a score of 84. Conclusion. A new fast, simple and green, but selective, accurate, precise and robust HPLC-UV method for simultaneous determination of valsartan and atenolol in newly formulated dosage form was developed and many possible variations of the same were suggested. The developed method for the simultaneous quantification of valsartan and atenolol in their challenging binary mixture offers simplicity essential for quality control of a large number of samples in short time intervals, which is necessary for routine analysis. The method was subjected to greenness profile assessment.
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Koot, M. J., F. N. Ijdenberg, R. M. Stuurman, J. Poell, L. J. Bras, J. J. M. Langemeijer, and L. Huen. "High pressure liquid chromatographic analysis of the serum concentration of cefuroxime after an intravenous bolus injection of cefuroxime in patients with a coronary artery bypass grafting." Pharmaceutisch Weekblad Scientific Edition 14, no. 6 (December 1992): 360–64. http://dx.doi.org/10.1007/bf01970173.
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Shulyak, N. S., A. D. Abbeyquaye, and D. B. Koval. "ROBUSTNESS EVALUATION OF HPLC DETERMINATION OF ATORVASTATIN AND LISINOPRIL ON COLUMN PUROSPHER C8 STAR IN PHARMACEUTICALS." Medical and Clinical Chemistry, no. 1 (May 22, 2021): 21–26. http://dx.doi.org/10.11603/mcch.2410-681x.2021.i1.12104.
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Introduction. Innovative pharmaceutical development of various antihypertensive drugs with statins and the creation of domestic fixed-dose combinations of drugs with different effects is an urgent task of modern pharmacy, which will help attract more patients to the treatment and prevention of cardiovascular disease. Pharmaceutical development of atorvastatin and lisinopril by our scientific group proposes for using the ratio of (1/1) for lisinopril (10 mg) and atorvastatin (10 mg). HPLC (High-Performance Liquid Chromatography) technique is adopted as it is considered as the most common technique in realm of quality control analysis.
The aim of the study – to evaluate the robustness of HPLC (High-Performance Liquid Chromatography) method for the quantitation of lisinopril and atorvastatin and determine the analytical parameters that present greater influence in the final results of the analysis.
Research Methods. An efficient method to assess the robustness of analytical methods is by Youden’s test, by means of an experiment design which involves seven analytical parameters combined in eight tests. In the recent studies, we assessed the robustness of a chromatographic method to quantify lisinopril and atorvastatin in tablets using Youden’s test.
Results and Discussion. By using the criteria of Youden’s test, HPLC method proved to be greatly robust regarding content of lisinopril and atorvastatin, when variations in seven analytical parameters were introduced. The most variation in effects of the analytical parameters in retention time (Rt) for lisinopril and atorvastatin HPLC quantitation was when used column supplier. Purospher C8 STAR (55 mm x 4mm, 5 μm) is based on high purity silica and an almost complete surface coverage. Purospher C8 STAR provides excellent peak symmetry for acidic, basic and even chelating compounds, highest column efficiency in terms of the number of theoretical plates, and exceptional stability from pH 1.5 to 10.5.
Conclusion. Youden’s test can be applied successfully for the robustness evaluation in validation process of analytical methods and results ontained in our work should be interest to the scientific population dealing with pharmaceutical analytical chemistry.
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Lonca, Nelly, Fabienne Maillard, Géraldine Leguelinel, Tahmer Sharkawi, and Ian Soulairol. "Validation of an HPLC Assay Method for Routine QC Testing and Stability Study of Compounded Low-Dose Capsules of Acetylsalicylic Acid." Pharmaceutical Technology in Hospital Pharmacy 3, no. 4 (November 27, 2018): 199–206. http://dx.doi.org/10.1515/pthp-2018-0022.
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Abstract Background The intolerance to Acetylsalicylic Acid (ASA) can be detected by conducting oral provocation testing (OPT), which is to gradually introduce low doses of ASA. To perform this test, hospital pharmacies compound small batches of different low-dosage ASA capsules. This work aims to validate a method for fast HPLC-UV assay that allows routine quality control and physicochemical stability studies of capsules. Methods The chromatographic separation is performed using a C18 column Kinetex (100 A, 50×4.6 mm, 2.6 µm) equipped with a precolumn C18. Separation is achieved using a mobile phase composed of water-acetonitrile-orthophosphoric acid (68:32:0.2 v/v/v) at a flow rate of 0.8 mL/min and UV detection at 237 nm. Results Validation shows that the method was suitable for routine analysis and could be used to perform stability studies. Conclusions The 5, 25, 100 and 250 mg dosed capsules show acceptable stability over 12 months, while the 1 mg dosed capsule show an unacceptable degradation of more than 15 % after 3 months. Therefore, hospital pharmacy can plan the manufacture of capsules and anticipate the requests of doctors.
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Chowdhury, Akhtaruzzaman, Md Ashraful Alam, Md Shafiullah Shajib, Mohammad Abdullah Al Mansur, and Mohammad A. Rashid. "Chemical Constituents and Protection of Biodiversity of Corypha taliera Roxb., a Critically Endangered Plant of Bangladesh." Bangladesh Pharmaceutical Journal 20, no. 2 (August 14, 2018): 213–20. http://dx.doi.org/10.3329/bpj.v20i2.37888.
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This article focuses on the chemical constituents and protection of biodiversity through plantation of saplings of Corypha taliera Roxb., a critically endangered plant of Bangladesh. Until 2010, the tree in the campus of University of Dhaka, used to be considered as the lone surviving species in the world in nature. Succesive chromatographic separation and purification of the methanol extract of air dried flowers of C. taliera provided β-sitosterol (1), β-amyrin (2), and betulinic acid (3) for the first time from its flowers. The structures of these purified compounds were established by extensive spectroscopic analysis and comparison of spectral data with published values as well as co-TLC with authentic samples. On the other hand, 500 mature seeds were sown in seed beds in the Medicinal Plant Garden of Faculty of Pharmacy, University of Dhaka, and Azimpur Government Officers' Quarter premises. After 40 days, the root was first seen to grow in its habitat and 85 days later the shoot developed up to 2.5 cm in height. The rate of germination was found to be 89-93%. The produced saplings were later on planted in different places of Bangladesh for conservation of the plant and protection of biodiversity by ex situ arrangement.Bangladesh Pharmaceutical Journal 20(2): 213-220, 2017
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Hecq, Jean-Daniel, Laurence P. Boitquin, Danielle F. Vanbeckbergen, Jacques Jamart, and Laurence M. Galanti. "Effect of the Freezing Conditions and Microwave Thawing Power on the Stability of Cefuroxime in Dextrose 5% Infusion Polyolefin Bags at 4 °C." Annals of Pharmacotherapy 39, no. 7-8 (July 2005): 1244–48. http://dx.doi.org/10.1345/aph.1e686.
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BACKGROUND Intravenous cefuroxime sodium solution could be prepared in advance by a centralized hospital pharmacy service to improve safety and time management. OBJECTIVE To investigate the effect of freezing and microwave thawing on the solution stability of cefuroxime. METHODS Cefuroxime 1.5 g in 100 mL of dextrose 5% in polyolefin bags was frozen individually (group A) or in one package (group B) for 98 days at −20 °C. The solutions were then thawed using microwaves at 270 (light cycle) or 800 watts (hard cycle) and stored at 4 °C. The cefuroxime concentration was measured by HPLC. Visual inspection was performed and pH was measured at that time. Stability of the solution was defined as a concentration remaining superior to 90% of the initial concentration by regression analysis. RESULTS No color change or precipitation in the solutions was observed. In group A, stability was at least 23 and 21 days after light and hard cycle thawing, respectively. In group B, stability was at least 21 and 18 days, respectively, with the pH increasing without affecting chromatographic parameters. CONCLUSIONS The optimal conditions for advance preparation of a solution containing cefuroxime 1.5% in dextrose 5% may be freezing of individual containers followed by a light cycle of microwave thawing.
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Melikyan, S., N. Biront, O. Pazderska, G. Mysko, M. M. Shymko, and D. Yanovych. "DEVELOPMENT OF THE METHOD FOR QUANTITATIVE DETERMINATION OF ENROFLOXACIN AND CYPROFLOXACIN IN CHICKEN SERUM USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH FLUOROMETRIC DETECTION." Scientific and Technical Bulletin оf State Scientific Research Control Institute of Veterinary Medical Products and Fodder Additives аnd Institute of Animal Biology 21, no. 2 (October 27, 2020): 110–17. http://dx.doi.org/10.36359/scivp.2020-21-2.15.
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Since Ukraine is a member of the World Trade Organization, so it has necessitated the transition of the entire veterinary drugs pharmacy industry to European and world levels and quality standards. Thus, a bill was approved this year which amended the process of state registration of veterinary drugs in the country. Therefore, the developed method is intended for clinical and pharmaceutical studies of veterinary drugs based on the active substances enrofloxacin and its main metabolite ciprofloxacin. Target analytes were extracted from the sample using the extraction by dichloromethane for 15 minutes, concentrated by drying and degreased with hexane/carbon tetrachloride. The procedure of sample preparation of fortified blood serum to construct calibration graphs is described in the manuscript. The mobile phase in the chromatographic separation consisted of acetonitrile and citrate buffer solution. The gradient mode of eluents was used during 16 min at a flow rate of 1.5 ml/min. Ciprofloxacin retention time is 8.80 min, and enrofloxacin retention time is 10.45 min. The validation parameters of the method were considered in accordance with the criteria of Council Directive 2002/657/EC and the Eurachem Guide. The specificity of the analytical technique was checked by chromatographic separation of serum sample spiked with enrofloxacin and ciprofloxacin mixture at the concentration of 20 μg/l and blank serum sample. The method is linear in the concentration range of 5.0 - 50.0 μg/l of each analyte. The results obtained in the study of the linearity of this technique were used to estimate the correctness and convergence. The accuracy of the measurements was evaluated by examining the known amounts of analytes added to the control serum samples. Recovery data are acceptable because they are within ± 10% of the target value. The method has sufficient convergence (accuracy). The evaluation of the intermediate accuracy of enrofloxacin and ciprofloxacin was assessed on three different days of analysis. The main advantages of the developed method are high selectivity and high sensitivity. The limit of detection for enrofloxacin is 0.05 μg/l, and for ciprofloxacin it is 0.02 μg/l, which competes with previously published HPLC/FLD methods for the determination these quinolones.
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Keevil, B. G., P. W. Maylor, and D. Rowlands. "A Rapid Anion Exchange High-Performance Liquid Chromatography Method for the Measurement of HbA2 in Whole Blood." Annals of Clinical Biochemistry: International Journal of Laboratory Medicine 33, no. 3 (May 1996): 253–56. http://dx.doi.org/10.1177/000456329603300313.
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We developed a binary gradient high-performance liquid chromatography (HPLC) method for measuring HbA2 in whole blood samples using a Pharmacia Mono Q column (1 mL) and measurement at 415 nm. The assay requires a simple lysis and centrifugation step before injection onto the column. We found good agreement of results between the HPLC method and the Helena column chromatography method. The within batch precision was 2·6% and between batch precision was 4·6%. We found that using 30 mM Tris buffers (pH 7·8) with a sodium chloride gradient resulted in short analysis times and good chromatographic separation of HbA2, HbS and HbA. We conclude that this is a robust assay for the diagnosis of β-thalassaemia.
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Peleshok, K. Y. "QUALITY CONTROL MEASUREMENT AND IN VITRO BIOEQUIVALENCE OF VALSARTAN AND ATENOLOL TABLETS MARKETED IN UKRAINE." International Journal of Medicine and Medical Research 6, no. 2 (May 18, 2021): 52–58. http://dx.doi.org/10.11603/ijmmr.2413-6077.2020.2.12013.
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Background. The urgent issue of hypertension is determined by its high population incidence, significant burden of the disease, risk of disability and impact on life expectancy. Rational combinations of drugs of different pharmacological groups in case of ineffectiveness of monotherapy to achieve the clinical effect of pharmacotherapy are clearly recommended in the world and national recommendations for diagnosis and treatment of hypertension. Therefore, innovative pharmaceutical development of a combination of antihypertensive drugs and creation of domestic drugs with antihypertensive action is an urgent task of contemporary pharmacy.
Objective. The aim of this study was to perform the quality control measurements and evaluation of dissolution tests for different brands of valsartan and atenolol tablets available in Ukraine.
Methods. The concentrations of valsartan and atenolol in samples (drug content and dissolution study) were determined by the proposed HPLC method.
Results. The results of the tests conducted for evaluation of the tablets were found to be in acceptable limits for all the selected brands. The correlation coefficient (R2) was 0.9991 and the regression equation was y=61.39x+0.3117. It has been established that the equivalence of dissolution profiles for all recommended dissolution media is observed (рН 1.2, 4.5, and 6.8) for the studied drugs. In all three dissolution media, the release rates of valsartan and atenolol of all dosage forms are more than 85% in 15 min. The dissolution profile of all the selected brands was within the standard limits and was acceptable.
Conclusions. Analytical method development is an integral part of the quality control measurements and evaluation of dissolution tests. Our previously developed HPLC method is essential for quality control of a large number of samples in short time intervals. Therefore, the method developed by our group is suitable for a routine quality control analysis of any pharmaceutical preparation containing two tested drugs with the suggested chromatographic method advantages for checking quality during dissolution studies of their dosage forms.
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Burda, Nadiia, Iryna Zhuravel, Moeen F. Dababneh, Andrii Kotov, Elina Kotova, and Andrii Popyk. "Identification and quantitative analysis of furostanol glycosides in caltrop." Pharmacia 67, no. 4 (October 2, 2020): 187–91. http://dx.doi.org/10.3897/pharmacia.67.e37433.
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This study describes the identification and quantitative determination of furostanol glycosides in caltrop herb harvested in the fructification period. Furostanol glycosides were identified by thin-layer chromatography (TLC) and quantified by UV-vis spectrophotometry. The furostanol glycosides were visualized on the TLC plate as pink spots after treatment with dimethylamine benzaldehyde solution. UV-vis spectrophotometry quantified these substances to the amount of at least 0.4 %. The data on the identification and quantification of furostanol glycosides obtained in the course of this research was implemented in the development of the Ukrainian State Pharmacopoeia for caltrop herb.
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Burda, Nadiia Ye, Iryna O. Zhuravel, Moeen F. Dababneh, and Yulia A. Fedchenkova. "Analysis of diosgenin and phenol compounds in Tribulus terrestris L." Pharmacia 66, no. 2 (July 9, 2019): 41–44. http://dx.doi.org/10.3897/pharmacia.66.e35023.
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Caltrop (Tribulusterrestris L.) is a weed plant widely growing in warm climate. The crude caltrop has multidirectional pharmacological action favorable for the development of drug preparations. As in European countries caltrop is a non-officinal plant, it seems feasible to develop raw material standardization parameters for creation of novel drugs. In the course of thin layer chromatography research the following compounds were identified in caltrop herb purveyed during the fruiting season: rutin, chlorogenic acid, caffeic acid, diosgenin. Diosgenin content in this raw material was determined by densitometry to be min. 0,11%.
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Logoyda, Liliya. "HPLC-MS/MS method development for the quantitative determination of nifedipine for Caco-2 permeability assay." Pharmacia 67, no. 2 (July 31, 2020): 83–88. http://dx.doi.org/10.3897/pharmacia.67.e50159.
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Aim. Poorly water-soluble drugs such as nifedipineoffer challenging problems in drug formulation as poor solubility is generally associated with poor dissolution characteristics and thus with poor oral bioavailability (BCS class II drugs). Methods of quantitative determination of nifedipine by methods of spectrophotometry and chromatography are described in the scientific literature. However, methods are not developedfor examination of nifedipine from Caco-2 cell monolayers. Caco-2 cell monolayers have been extensively used for years as a tool to test permeability, assess the oral absorption potential and study the absorption mechanism of compounds. Therefore, the aim of this study was to develop and validate an efficient HPLC MS/MS method for determination of nifedipine from Caco-2 cell monolayers. Materials and methods. Chromatography was achieved on DiscoveryC18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile – water – formic acid, 5 : 95 : 0.1 v/v), eluent B (acetonitrile – formic acid, 100 : 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.4 mL/min into the mass spectrometer ESI chamber. The sample volume was 5 μl. Results. Under these conditions, nifedipine was eluted at 1.83 min. A linear response function was established at 1 – 100 ng/mL. The regression equation for the analysis was Y = 0.0323x-0.00121 with coefficient of correction (R2) = 0.9987. According to the Caco-2 test results, nifedipine showed high permeability. The within-run coefficients of variation ranged between 0.331% and 0.619% for nifedipine. The within-run percentages of nominal concentrations ranged between 98.80% and 100.63% for nifedipine. The between-run coefficients of variation ranged between 0.332% and 0.615% for nifedipine. The between-run percentages of nominal concentrations ranged between 98.98% and 101.71% for nifedipine. The assay values on both the occasions (intra- and inter-day) were found to be within the accepted limits. Conclusion. From results of analysis, it can be concluded that developed method is simple and rapid for determination of nifedipine from confluent Caco-2 monolayers and from aqueous solution. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for examination of nifedipine from Caco-2 cell monolayers.
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Natrus, L. V., O. I. Kryvosheyeva, G. R. Lamazyan, and T. S. Bruzgina. "EFFECT OF MODIFICATION OF THE EXTRACTION TECHNIQUE OF THE SUBSTANCE IN A SOXHLET FOR CONTENT OF FATTY ACIDS." Journal "Medical Science of Ukraine" (NMU) 14, no. 1-2 (June 21, 2018): 18–23. http://dx.doi.org/10.32345/1998-3719.1-2.2018.03.
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Relevance. The search for new forms of herbal medicine is an important area of modern biotechnology, pharmacology and pharmacy. More and more attention is paid to the development of extracts from plant materials, since the extraction products provide the maximum content of biologically active substances, which increases the rationality of their use, due to the accuracy of dosing, the therapeutic effect is increased, the period of use increases and storage conditions are simplified. The extraction of the fruit mixture of Citrullus сolocynthis in the Soxhlet apparatus was modified by reducing the procedure time 5-10 times and improving the processing of raw materials by using a press at the same time and increasing the temperature, or even by modifying the apparatus.
Objective: to study the composition of FA in an aqueous solution of the dry extract of Citrullus сolocynthis when modifying the extraction mixture in the Soxhlet apparatus by increasing the temperature and technological reduction of processing time.
Materials and methods. We carried out the determination and comparison of the composition of FA’s by gas-liquid chromatography of all parts of the fruit of Citrullus сolocynthis and in an aqueous solution of its dry extract with various concentrations of the substance.
Results. Chromatographic analysis showed that all parts of the fetus Citrullus colocynthis are promising sources of saturated and unsaturated FA. In all parts of the fruit of Citrullus colocynthis, linoleic acid prevails in quantitative content. The modification of the extraction of the mixture in the Soxhlet apparatus by increasing the temperature and technological reduction in the processing time of the raw materials led to the production of a substance with a new composition and FA content. The ratio of unsaturated / saturated FA in the resulting dry extract is 5 times greater than the similar ratio separately in seeds, pulp and shell. At the same time, the distribution of separate unsaturated and polyunsaturated FA’s in the dry extract solution is fairly uniform. The relative amount of linoleic FA in the dry extract was smaller, and the linolenic FA was greater than in the seeds and pulp of the fruit.
Conclusions. Modifying the extraction of the mixture in the Soxhlet apparatus by increasing the temperature and technological reduction of the processing time did not lead to complete degreasing of the substrate and allowed to obtain a dry extract of Citrullus solvent with content of microdoses of the FA, their balanced (uniform) in amount, and predominance of 5 times the amount of unsaturated polyunsaturated FA over the amount of saturated. We assume that such a redistribution of FA, and especially their micro doses, can be the basis for creating medicines with more effective effects on the body.
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Natrus, L. V., O. I. Kryvosheyeva, G. R. Lamazyan, and T. S. Bruzgina. "EFFECT OF MODIFICATION OF THE EXTRACTION TECHNIQUE OF THE SUBSTANCE IN A SOXHLET FOR CONTENT OF FATTY ACIDS." Medical Science of Ukraine (MSU) 14, no. 1-2 (June 21, 2018): 18–23. http://dx.doi.org/10.32345/2664-4738.1-2.2018.03.
Full textAbstract:
Relevance. The search for new forms of herbal medicine is an important area of modern biotechnology, pharmacology and pharmacy. More and more attention is paid to the development of extracts from plant materials, since the extraction products provide the maximum content of biologically active substances, which increases the rationality of their use, due to the accuracy of dosing, the therapeutic effect is increased, the period of use increases and storage conditions are simplified. The extraction of the fruit mixture of Citrullus сolocynthis in the Soxhlet apparatus was modified by reducing the procedure time 5-10 times and improving the processing of raw materials by using a press at the same time and increasing the temperature, or even by modifying the apparatus.
Objective: to study the composition of FA in an aqueous solution of the dry extract of Citrullus сolocynthis when modifying the extraction mixture in the Soxhlet apparatus by increasing the temperature and technological reduction of processing time.
Materials and methods. We carried out the determination and comparison of the composition of FA’s by gas-liquid chromatography of all parts of the fruit of Citrullus сolocynthis and in an aqueous solution of its dry extract with various concentrations of the substance.
Results. Chromatographic analysis showed that all parts of the fetus Citrullus colocynthis are promising sources of saturated and unsaturated FA. In all parts of the fruit of Citrullus colocynthis, linoleic acid prevails in quantitative content. The modification of the extraction of the mixture in the Soxhlet apparatus by increasing the temperature and technological reduction in the processing time of the raw materials led to the production of a substance with a new composition and FA content. The ratio of unsaturated / saturated FA in the resulting dry extract is 5 times greater than the similar ratio separately in seeds, pulp and shell. At the same time, the distribution of separate unsaturated and polyunsaturated FA’s in the dry extract solution is fairly uniform. The relative amount of linoleic FA in the dry extract was smaller, and the linolenic FA was greater than in the seeds and pulp of the fruit.
Conclusions. Modifying the extraction of the mixture in the Soxhlet apparatus by increasing the temperature and technological reduction of the processing time did not lead to complete degreasing of the substrate and allowed to obtain a dry extract of Citrullus solvent with content of microdoses of the FA, their balanced (uniform) in amount, and predominance of 5 times the amount of unsaturated polyunsaturated FA over the amount of saturated. We assume that such a redistribution of FA, and especially their micro doses, can be the basis for creating medicines with more effective effects on the body.
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Logoyda, Liliya, Marjan Piponski, Sergiy Kovalenko, Olha Denefil, Olha Dutchak, Yuriy Soroka, Svitlana Pidruchna, Dariya Popovych, and Oleksandr Susla. "Method development for the quantitative determination of captopril from Caco-2 cell monolayers by using LC-MS/MS." Pharmacia 68, no. 1 (January 7, 2021): 61–67. http://dx.doi.org/10.3897/pharmacia.68.e52077.
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Aim. Caco-2 cells are a human colon epithelial cancer cell line used as a model of human intestinal absorption of drugs and other compounds. Although compounds were used in the original Caco-2 cells monolayer assays, compounds have been replaced in most laboratories by the use of liquid chromatography-mass spectrometry (LC-MS) and LC-tandem mass spectrometry (LC-MS/MS). Mass spectrometry not only eliminates the need for compounds, but permits the simultaneous measurement of multiple compounds. The measurement of multiple compounds per assay reduces the number of incubations that need to be carried out, thereby increasing the throughput of the experiments. Furthermore, LC-MS and LC-MS-MS add another dimension to Caco-2 assays by facilitating the investigation of the metabolism of compounds by Caco-2 cells. A simple, rapid LC-MS/MS method has been developed for determination of captopril from confluent Caco-2 monolayers and from aqueous solution. Materials and methods. Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile – water – formic acid, 5 : 95 : 0.1 v/v), eluent B (acetonitrile – formic acid, 100 : 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.4 mL/min into the mass spectrometer ESI chamber. The sample volume was 5 μl. Results. Under these conditions, captopril was eluted at 1.42 min. A linear response function was established at 2 – 200 ng/mL. The regression equation for the analysis was y =0.0187x+0.000248 with coefficient of correction (r2) = 0.9993. According to the Caco-2 test results, captopril showed low permeability. It should be noted that the recovery value is 103.20%. The within-run coefficients of variation ranged between 0.321% and 0.541%. The within-run percentages of nominal concentrations ranged between 99.13% and 101.12%. The between-run coefficients of variation ranged between 0.314% and 0.663%. The between-run percentages of nominal concentrations ranged between 99.17% and 101.03%.The assay values on both the occasions (intra- and inter-day) were found to be within the accepted limits. Conclusion. From results of analysis, it can be concluded that developed method is simple and rapid for determination of captopril from confluent Caco-2 monolayers and from aqueous solution. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for examination of captopril from Caco-2 cell monolayers.
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NUNES, Luiz Fernando Mendes. "DETERMINING THE INFLUENCE OF CONDUCTIVITY IN ION CHROMATOGRAPHY ANALYSIS." Periódico Tchê Química 12, no. 24 (January 20, 2013): 42–46. http://dx.doi.org/10.52571/ptq.v11.n20-21.2013.42_periodico20e21_pgs_42_46.pdf.
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The conductivity of water for use in chromatography is a feature that deserves close attention when you want to express reliable analytical results. The objective of this paper is to present, through analytical testing that the conductivity of the reagent ion chromatography for water does not exert significant impact on the results of concentration and conductivity. The parameters evaluated were the anions fluoride, chloride, nitrate, phosphate and sulfate. The results indicate that the P3 pattern prepared with reagent water with a conductivity of 1.0 mS / cm and 9.8 mS / cm derived from mixed bed has the same behavior pattern P3 prepared with conductivity 0.7 mS / cm water. We conclude that the conductivity of the samples do not offer variations in the concentration of anions.
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Logoyda, Liliya, Maksym Herasymiuk, Dariya Popovych, Svitlana Pidruchna, Vitaliy Hlushok, Nazar Herasymiuk, and Nadiya Zarivna. "HPLC MS/MS method development for the quantitative determination of verapamil hydrochloride from Caco-2 cell monolayers." Pharmacia 67, no. 2 (July 31, 2020): 63–69. http://dx.doi.org/10.3897/pharmacia.67.e48896.
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Aim. An understanding of the role that transporters, in particular P-glycoprotein (P-gp), can play in the absorption, distribution, metabolism and excretion (ADME) of candidate drugs, and an assessment of how these processes might impact on toxicity and the potential for drug-drug interactions in the clinic, is required to support drug development and registration. It is therefore necessary to validate preclinical assays for the in vitro evaluation of candidate drugs as substrates or inhibitors of human P-gp. 2. A simple, rapid HPLC MS/MS method was developed for determination of verapamil hydrochloride from confluent Caco-2 monolayers and from aqueous solution. Materials and methods. Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile – water – formic acid, 5 : 95 : 0.1 v/v), eluent B (acetonitrile – formic acid, 100 : 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.4 mL/min into the mass spectrometer ESI chamber. The sample volume was 5 μl. Results. Under these conditions, verapamil hydrochloride was eluted at 1.08 min. A linear response function was established at 1 – 100 ng/mL. The regression equation for the analysis was Y = 0.0162x + 0.00391 with coefficient of correction (R2) = 0.9992. According to the Caco-2 test results, verapamil showed low permeability. It should be noted that the recovery value for verapamil hydrochloride is 102.69%. The within-run coefficients of variation ranged between 0.336% and 0.617% for verapamil. The within-run percentages of nominal concentrations ranged between 98.82% and 100.62% for verapamil. The between-run coefficients of variation ranged between 0.334% and 0.612% for verapamil. The between-run percentages of nominal concentrations ranged between 98.97% and 101.76% for verapamil. The assay values on both the occasions (intra- and inter-day) were found to be within the accepted limits. Conclusion. From results of analysis, it can be concluded that developed method is simple and rapid for determination of verapamil hydrochloride from confluent Caco-2 monolayers and from aqueous solution. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for examination of verapamil hydrochloride from Caco-2 cell monolayers.
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Shkondrov, Aleksandar, and Ilina Krasteva. "Liquid chromatography – high resolution mass spectrometry screening of Astragalus hamosus and Astragalus corniculatus." Pharmacia 68, no. 1 (January 8, 2021): 135–39. http://dx.doi.org/10.3897/pharmacia.68.e60621.
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Astragalus hamosus and Astragalus corniculatus were examined for the presence of flavoalkaloids, acylated and highly glycosylated flavonoids. Non-purified extracts of the overground parts of the species were subjected to ultra-high performance liquid chromatography – high resolution electrospray ionisation mass spectrometry (UHPLC-HRESIMS) analysis and the results were compared to authentic reference substances. A flavoalkaloid of kaempferol was newly identified in an extract of A. hamosus. In addition, three compounds – quercetin and kaempferol flavonoids, acylated with hydroxymethylglutaric acid and alcesefoliside, were found in extracts of A. hamosus and A. corniculatus for the first time.
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Shkondrov, Aleksandar, and Ilina Krasteva. "Liquid chromatography – high resolution mass spectrometry screening of Astragalus hamosus and Astragalus corniculatus." Pharmacia 68, no. 1 (January 8, 2021): 135–39. http://dx.doi.org/10.3897/pharmacia.68.e60621.
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Astragalus hamosus and Astragalus corniculatus were examined for the presence of flavoalkaloids, acylated and highly glycosylated flavonoids. Non-purified extracts of the overground parts of the species were subjected to ultra-high performance liquid chromatography – high resolution electrospray ionisation mass spectrometry (UHPLC-HRESIMS) analysis and the results were compared to authentic reference substances. A flavoalkaloid of kaempferol was newly identified in an extract of A. hamosus. In addition, three compounds – quercetin and kaempferol flavonoids, acylated with hydroxymethylglutaric acid and alcesefoliside, were found in extracts of A. hamosus and A. corniculatus for the first time.
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Philcox, J. C., M. R. Haywood, and A. M. Rofe. "Hemoglobin A1C by Hplc with the Pharmacia Mono S HR 5/N Cation-Exchange Column: Influence of Sample Protein Load on Optimal Chromatographic Conditions." Clinical Chemistry 38, no. 8 (August 1, 1992): 1488–90. http://dx.doi.org/10.1093/clinchem/38.8.1488.
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Abstract The Pharmacia Mono S HR 5/5 column has been optimized for hemoglobin A1c analysis by HPLC by using a much smaller column load, decreased buffer flow rate, and a steeper gradient than was used in previously described methods. Superior chromatographic separation, shorter analysis time, and a greatly extended column life have resulted.
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Dickenson, J. M., T. N. Huckerby, and I. A. Nieduszynski. "Two linkage-region fragments isolated from skeletal keratan sulphate contain a sulphated N-acetylglucosamine residue." Biochemical Journal 269, no. 1 (July 1, 1990): 55–59. http://dx.doi.org/10.1042/bj2690055.
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Peptido-keratan sulphate fragments were isolated from the nucleus pulposus of bovine intervertebral discs (6-year-old animals) after chondroitin ABC lyase digestion followed by digestion of A1D1 proteoglycans by diphenylcarbamoyl chloride-treated trypsin and gel-permeation chromatography on Sepharose CL-6B. Treatment of these peptido-keratan sulphate fragments with alkaline NaB3H4 yielded keratan sulphate chains with [3H]galactosaminitol end-labels, and these chains were further purified by gel-permeation chromatography on Sephadex G-50 and ion-exchange chromatography on a Pharmacia Mono-Q column in order to exclude any contamination with O-linked oligosaccharides. The chains were then treated with keratanase, and the digest was chromatographed on a Bio-Gel P-4 column followed by anion-exchange chromatography on a Nucleosil 5 SB column. Two oligosaccharides, each representing 18% of the recovered radiolabel, were examined by 500 MHz 1H-n.m.r. spectroscopy, and shown to have the following structures: [formula: see text] The structure of oligosaccharide (I) confirms the N-acetylneuraminylgalactose substitution at position 3 of N-acetylgalactosamine in the keratan sulphate-protein linkage region found by Hopwood & Robinson [(1974) Biochem. J. 141, 57-69] but additionally shows the presence of a 6-sulphated N-acetylglucosamine. Electron micro-probe analysis specifically confirmed the presence of sulphur in this sample. This sulphate ester group differentiates the keratan sulphate linkage region from similar structures derived from O-linked oligosaccharides [Lohmander, De Luca, Nilsson, Hascall, Caputo, Kimura & Heinegård (1980) J. Biol. Chem. 255, 6084-6091].
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Salo, Jukka-Pekka, and Hannele Salomies. "Teaching the Basics of Pharmaceutical Analysis by Thin-Layer Chromatography and High-Performance Thin-Layer Chromatography to Undergraduate Students—Laboratory Practicals." Journal of AOAC INTERNATIONAL 82, no. 1 (January 1, 1999): 38–47. http://dx.doi.org/10.1093/jaoac/82.1.38.
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Abstract As part of the renewal of the pharmacy students’ curriculum, we planned a 2-day program with 9 exercises in thin-layer chromatography to teach the basics of the technique. Written reports with proper presentation ofresults were required. Related issues such assimple experimental design were integrated into the program. The results and difficultiesin their interpretation are described from a teacher’s point of view. As in real life, some exercises do not allow simple conclusions or complete solutions to a problem. The mostly positive feedback about the program suggests the program served its purpose well.
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Popova, Pavlinka, Yancho Zarev, and Iliana Ionkova. "Biotransformation of quercetin, kaempferol and apigenin to monoglycosylated derivatives by in vitro suspension cultures of Astragalus vesicarius ssp. carniolicus." Pharmacia 68, no. 2 (April 1, 2021): 307–11. http://dx.doi.org/10.3897/pharmacia.68.e54289.
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Biotransformation of exogenous substrates quercetin, kaempferol and apigenin by suspension cultures of Astragalus vesicarius ssp. carniolicus to their monoglycosylated derivatives was performed. The maximal enzymatic potential of cells of A. vesicarius ssp. carniolicus was evaluated by different concentrations of substrate exposure. According to quantitative ultra-high performance liquid chromatography-high resolution electrospray ionization mass spectrometry (UHPLC-HR-ESI-MS) analysis, the highest concentration of kaempferol O-glycoside (14.88 nmol/g dry weight, DW), apigenin O-glycoside (10.55 nmol/g DW) and quercetin O-glycoside (150.83 nmol/g DW) was achieved, when suspension cultures were treated with 4 mg/mL kaempferol, 4 mg/mL apigenin and 3 mg/mL quercetin, respectively. The glycosidic products of biotransformation were not detected in the untreated control.
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Savych, Alona, Roksolana Basaraba, Nataliіa Muzyka, and Pavlina Ilashchuk. "Analysis of fatty acid composition content in the plant components of antidiabetic herbal mixture by GC-MS." Pharmacia 68, no. 2 (May 20, 2021): 433–39. http://dx.doi.org/10.3897/pharmacia.68.e66693.
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Medical plants and their combinations due to the wide range of biologically active substances can influence on various links of the pathogenetic mechanism of development of diabetes mellitus and its complications. One of such combinations is an anidiabetic herbal mixture (Urtica dioica L. leaf, Rosa majalis L. fruits, Vaccinium myrtillus L. leaf, Mentha piperita L. herb and Taraxacum officinale L. roots) with established hypoglycemic, hypolipidemic, antioxidant, hepatoprotective, pancreatoprotective activity in previous pharmacological study in vivo. Thus, the aim of this study was to identify and establish the fatty acid content in the plant components of antidiabetic herbal mixture. Fatty acids were separated by validated method of of gas chromatography-mass spectrometry after conversion into methyl esters. The result showed that Urtica dioica L. leaf and Vaccinium myrtillus L. leaf contain 12 fatty acids (8 saturated, 2 monounsaturated and 2 polyunsaturated), Rosa majalis L. fruits and Taraxacum officinale L. roots – 13 fatty acids (9 saturated, 2 monounsaturated and 2 polyunsaturated) and Mentha piperita L. herb – 14 fatty acids (10 saturated, 2 monounsaturated and 2 polyunsaturated). The predominant long-chain carboxylic acids in all plant raw materials were unsaturated fatty acids, their content was 55.3% in Urtica dioica L. leaf, 64.7% in Rosa majalis L. fruits, 60.5% in Vaccinium myrtillus L. leaf, 64.3% in Mentha piperita L. herb and 51.7% in Taraxacum officinale L. roots. This indicates the feasibility of including each component in the antidiabetic herbal mixture in order to form anticholesterolemic, anti-inflammatory, immunomodulatory and neuroprotective activity, due to the high content of omega-3, omega-6 and omega-9 fatty acids.
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Savych, Alona, Oksana Bilyk, Valentina Vaschuk, and Ihor Humeniuk. "Analysis of inulin and fructans in Taraxacum officinale L. roots as the main inulin-containing component of antidiabetic herbal mixture." Pharmacia 68, no. 3 (July 21, 2021): 527–32. http://dx.doi.org/10.3897/pharmacia.68.e66266.
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Herbs and their combinations due to the wide range of biologically active substances can influence on various links of the pathogenetic mechanism of development of diabetes mellitus and its complications. One of such combinations is an antidiabetic herbal mixture with established hypoglycemic, hypolipidemic, antioxidant, hepatoprotective, pancreatoprotective activity in previous pharmacological study in vivo that including an inulin-containing component – Taraxacum officinale L. roots. Thus, the aim of this study was to determine the quantitative content of inulin and fructans in Taraxacum officinale L. Quantity content of inulin was determined by the difference between fructose as a product of enzymatic hydrolysis and D-fructose, a constituent of sucrose and free D-fructose, taking into account the empirical factor for the conversion of D-fructose from inulin. Carbohydrates used in the calculation of inulin were separated by gas chromatography-mass spectrometry after conversion into volatile derivatives as aldononitrile acetate. According to the results, Taraxacum officinale L. roots contain 436.29 mg/g of inulin. Total content of fructans was determined by spectrophotometric analysis as a product of acid hydrolysis of 5-(hydroxymethyl)furfural. The results show that Taraxacum officinale L. roots contain 39.49% of fructans. The obtained results are evidence that this plant component should be included in the herbal antidiabetic mixture, because due to the presence of fructans and inulin causes hypoglycemic, hypolipidemic and detoxification activity.
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Larskiy, M. V., A. E. Pozdnyakova, Z. D. Khadzhieva, and D. I. Pozdnyakov. "DEVELOPMENT AND VALIDATION OF METHODS FOR QUANTITATIVE DETERMINATION OF ACTIVE PHARMACEUTICAL SUBSTANCES IN NASAL SPRAY." Pharmacy & Pharmacology 9, no. 4 (September 8, 2021): 266–77. http://dx.doi.org/10.19163/2307-9266-2021-9-4-266-277.
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Intranasal administration of H1-histamine receptor blockers may be a promising approach to the treatment of allergic rhinitis. Earlier, an original composition of a nasal spray containing fexofenadine hydrochloride and ammonium glycyrrhizinate and demonstrating a high level of therapeutic efficacy, was developed.The aim of the study was to develop and validate a method of the quantitative determination of active pharmaceutical ingredients fexofenadine hydrochloride and ammonium glycyrrhizinate in a spray for intranasal administration.Materials and methods. During the development and validation of the method of the fexofenadine hydrochloride and ammonium glycyrrhizinate quantitative determination in a nasal spray, the method of high performance liquid chromatography was used: a Dionex Ultimate 3000 UV chromatograph with a Luna C18 column (2) containing octadecylsilicagel with a 5 μm grain size as a sorbent. The analysis and validation procedures were performed in accordance with the requirements of the State Pharmacopoeia of the Russian Federation, the XIVth edition.Results. The study showed that for the simultaneous quantitative determination of fexofenadine hydrochloride and ammonium glycyrrhizinate, the optimal elution regime is a gradient mode with a mobile phase containing 50 mmol/L potassium dihydrogen phosphate solution with methanol (45:55), which ensured the separation of the components in the 20 minutes interval. The validation procedures showed that the developed methodology correspond to all the criteria of validity in terms of the following indicators: correctness, precision, specificity and linearity in the analytical area.Conclusion. The obtained results indicate the possibility of using the method of high-performance liquid chromatography in a gradient elution mode with a mobile phase of the composition of a 50 mmol/L solution of potassium dihydrogen phosphate with methanol (45:55) for the simultaneous quantitative determination of active pharmaceutical ingredients – fexofenadine hydrochloride and ammonium glycyrrhizinate as parts of a promising nasal spray for the allergic rhinitis treatment.
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VILLA, Sabrina Moura, Thamiris Brandino STELLATO, Joyce Rodrigues MARQUES, Mainara Generoso FAUSTINO, Douglas Batista SILVA, Lucilena Rebelo MONTEIRO, Tatiane B. S. Carvalho DA SILVA, Marycel E. Barbosa COTRIM, and Maria Aparecida F. PIRES. "QUALITY ASSURANCE OF ANIONS ENVIRONMENTAL MONITORING IN IPEN S ENVIRONMENTAL MONITORING PROGRAM." Periódico Tchê Química 14, no. 27 (January 20, 2017): 91–96. http://dx.doi.org/10.52571/ptq.v14.n27.2017.90_periodico27_pgs_91_96.pdf.
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This work aims to assess the internal and external quality control of the anion analysis, accomplished at IPEN, using chromatography technique ions and Statistical Methods for data analysis. So it was possible to conclude that the system is over control, generating reliable results
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Petrova, Svetla, and Valentina Christova-Bagdassarian. "Analytical difficulties for determination of acesulfame K in chocolate products." Pharmacia 67, no. 2 (August 6, 2020): 105–10. http://dx.doi.org/10.3897/pharmacia.67.e55257.
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Sweeteners are substances used as a dietary supplement to replace sugar. Consumers are concerned about the high levels of sugar, calories and cariogenicity in confectionery products, which is why the popularity of the so-called. „Light“ products and „sugar-free“ products. Acesulfame K is a synthetic sweetener about 200 times sweeter than sugar. In the present work, an analysis of acesulfame K in cocoa and chocolate products was performed. For the determination of sweeteners acesulfame K, saccharin and aspartame in foodstuffs, a standardized reverse phase high performance liquid chromatography method with UV detection was used. A cocoa matrix-specific compound was observed in all chocolate products analyzed for acesulfame K. Interference did not correspond to acesulfame K on the UV spectrum and could not be removed by two-step purification. The comparison of the spectral characteristics allowed to avoid a misleading result for the presence of acesulfame K in chocolate and cocoa products.
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Kumar, Lokesh, Prakash Kumbhar, and Janhavi Patharkar. "Pharmaceutical Analysis of Guduchi-Bhadramustadi Ghanvati: An Ayurvedic Formulation for Dyslipidemia." International Journal of Ayurvedic Medicine 12, no. 1 (March 31, 2021): 144–47. http://dx.doi.org/10.47552/ijam.v12i1.1808.
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Ayurveda a science life which deals the maintenance of health and treatment for the diseases manifested in the human body. In Ayurveda many herbal and herbo-mineral formulations have been explained for disease treatment. Guduchi-Bhadramustadi yoga is herbal formulation explained in classical which consists of five herbal medicines and it has been converted in to Ghanavati form by following the sop in GMP certified pharmacy. It is a classical preparation used in the management of Kapha Dosha Vikaras by practitioners. Material & Methods: The present study was aimed to recognize the constituents of Guduchi-Badraustadi Ghanavati by using physico-chemical parameters, Qualitative analysis and Chromatography (HPTLC). Conclusion: This study will be useful for standardization of Guduchi-Badramustadi Ghanavati and for the preparation of the monography of this formulation for the Ayurvedic Formulary of India (AFI).
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Savych, Alona, Svetlana Marchyshyn, Myroslava Harnyk, Victoria Kudria, and Anna Ocheretniuk. "Determination of amino acids content in two samples of the plant mixtures by GC-MS." Pharmacia 68, no. 1 (March 15, 2021): 283–89. http://dx.doi.org/10.3897/pharmacia.68.e63453.
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Due to the wide range of biologically active substances, the plant mixtures can influence the development of diabetes mellitus and its complications. Amino acids attract particular attention due to their ability to stimulate insulin secretion, reduce hyperglycemia and regulate metabolic processes in patients with diabetes. The aim of this study was to investigate the content of amino acids in the plant mixture samples: 1) Cichorium intybus roots, Elymus repens rhizome, Helichrysum arenarium flowers, Rosa majalis fruits, Zea mays columns with stigmas, 2) Urtica dioica leaf, Taraxacum officinale roots, Vaccinium myrtillus leaf, Rosa majalis fruits, Mentha piperita herb, which have proven antidiabetic activity in studies in vivo. The amino acids were separated by validated method of gas chromatography-mass spectrometry with pre-column derivatisation. Quantitative analyses of amino acids showed that the predominant components were L-proline in the sample 1 and L-leucine and L-proline in the sample 2 of the plant mixtures.
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ALMEIDA, M. S., A. C. GOULART, S. M. GOULART, T. A. da SILVA, and J. P. V. SANTOS. "ANALYSIS OF ALDICARB IN SURFACE WATER FROM THE PARANÁIBA RIVER." Periódico Tchê Química 15, no. 29 (January 20, 2018): 31–38. http://dx.doi.org/10.52571/ptq.v15.n29.2018.31_periodico29_pgs_31_38.pdf.
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The pesticide aldicarb is the most toxic active ingredient registered in all national territory, standing out for its extreme acute toxicity. In the environment, mainly in the water resources, several studies have demonstrated the potential of contamination of aldicarbe. The Paranaíba River cuts off the municipality of Itumbiara-GO, a region considered an important economic center in the south of the state. Along the Paranaíba River Basin there is a wide range of crops, such as sugarcane, corn, soy, cotton. This work aimed to quantitatively analyze the occurrence of aldicarb contamination in surface waters of the Paranaíba River, in addition to conducting a theoretical study of the river. For this purpose, the liquidliquid extraction with low temperature partitioning (LLE-LTP) and high-performance liquid chromatography (HPLC-UV) analysis were used. In the surface water samples of the river analyzed, no aldicarb contamination levels were found or the concentrations were below the detection limit of the LLE-LTP and HPLC-UV method.
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Marehn, David Thomas, Detlef Wilhelm, Heike Pospisil, and Roberto Pizzoferrato. "Proving the Preclusion of Data Manipulation Using Parallel Data Acquisition in Chromatography." Materials Science Forum 941 (December 2018): 2390–94. http://dx.doi.org/10.4028/www.scientific.net/msf.941.2390.
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Traceability has an enormous value for companies, but especially for those working in the regulated environment. It plays a special role in the field of pharmacy with respect to manufacturing, controlling and distributing batches of drugs. Through the guidance of Good Manufacturing Practice (GMP) traceability should be ensured. An increasing number of pharmaceutical companies are member of one of the global pharmacopoeias (United States Pharmacopeia, European Pharmacopeia and Japanese Pharmacopeia). The specifications of these pharmacopoeias describe the best practice in documentation, control, qualification and risk management. But however, the pharmacopoeias are written very generally and do not distinguish between the vendors of the analytical instruments. Here, we analyze how chromatographic analyses and data acquisition rely on a specific vendor of the device and the chromatography data system (CDS), the controlling software. We present a way to compare the data acquisition of different CDSs communicating with HPLC instruments. A newly developed software called Data Collector allows the acquisition of data from a HPLC detector parallel to the controlling CDS in the same run. Two HPLC systems and two different CDSs using a well defined sample standard have been tested. The direct comparison of the acquired data precludes unexpected data manipulations of both tested CDSs and shows that there are primarily deviations between the CDSs due to time variations only which depend on the sampling rate. All in all the Data Collector can be used for the traceability of data acquisition.
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SALIKOVA, Natalya S., Ainash U. BEKTEMISSOVA, Valentina D. NAZAROVA, Bahyt E. BEGENOVA, and Natalya V. OSTAFEICHUK. "ISOLATION OF MIRICETINE-CONTAINING FRACTIONS FROM LINOSYRIS VILLOSA PLANT AND THEIR APPLICATION AS ANTIANEMIC AGENT." Periódico Tchê Química 17, no. 35 (July 20, 2020): 998–1012. http://dx.doi.org/10.52571/ptq.v17.n35.2020.82_nazarova_pgs_998_1012.pdf.
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With the development of chemistry, natural substances were actively supplanted from human life by chemical products. However, despite the enormous progress in this area, in recent decades, the problems of serious side effects of synthetic chemicals on the environment have become more and more pronounced. Methods of two-dimensional and one-dimensional paper chromatography, column adsorption chromatography, gas chromatography, and IR spectroscopy were used. The purpose of the article is to study the chemical composition of the Linosyris villosa plant by physicochemical methods of analysis. Creation of dosage forms based on it. The problem of the article is the search and creation of drugs based on the flora of Northern Kazakhstan. The scientific novelty lies in the fact that the chemical composition and biological activity of the Linosyris villosa plant, growing in the territory of Northern Kazakhstan, is being studied for the first time. According to the results of the analysis, in 13% of patients the treatment effect is insignificant, and in 87% of patients there was an improvement in blood values (increase in hemoglobin, an increase in the number of red blood cells, almost all patients returned color index of blood), the number of white blood cells increased to normal, and the WBC differential improved. Therefore, the drug “Vitin”, an aqueous-alcoholic extract of the Linosyris villosa, is an effective drug for the treatment of patients with anemia of varying severity. The practical significance of the work is defined as follows: biologically active compounds from the Linosyris villosa plant were obtained for the purpose of studying and applying them in medicine and agriculture.
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Sytryn, Anastasiia, Iryna Cholak, Oksana Yemelianova, and Uliana Karpiuk. "Pharmacognostic analysis of Salvia hispanica L. seeds." ScienceRise: Pharmaceutical Science, no. 2 (30) (April 30, 2021): 49–54. http://dx.doi.org/10.15587/2519-4852.2021.230290.
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The aim. The aim of this work was to conduct a microscopic and phytochemical study of the seeds of chia (Salvia hispanica L.).
Materials and methods. Chia seeds were examined macroscopically and microscopically. To study the qualitative composition of the main groups of biologically active substances, histochemical, microchemical and chemical reactions were used. Hydroxycinnamic acids were identified by paper chromatography. To obtain a lipophilic extract, a Soxhlet apparatus and an exhaustive chloroform extraction method were used. The study of the quantitative content of fatty acids was carried out by gas chromatography. The content of polysaccharides in the raw material was determined by the gravimetric method. According to the SPhU method, the raw material swelling index was determined.
Results. The main macro- and microscopic features of chia seeds have been established. Histochemical reactions, microchemical reactions made it possible to establish the presence of mucus and fatty oils in chia seeds. With the help of chemical reactions, the presence of flavonoids in the raw material was established. The quantitative content of fatty oils is 24.0±1.2 %. The content of water-soluble polysaccharides in the whole raw material was 4.01±0.07 %, in the crushed raw material - 5.04 ± 0.05 %. As a result of determining the swelling index, it was found that this indicator for the whole chia seeds was 20, and for the crushed ones – 17. The content of hydroxycinnamic acids in the chia seeds was 1.07±0.03 %. 9 fatty acids have been identified, among which linoleic acid predominates in terms of content.
Conclusions. The presence and quantitative content of mucus, fatty oils, water-soluble polysaccharides, flavonoids, hydroxycinnamic acids, fatty acids was confirmed in the seeds of chia (Salvia hispanica L.). The obtained data can be used to develop regulatory documentation for chia seeds in order to use this raw material in pharmacy and medicine
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Seckute, Jolita, Ingrid Castellanos, and Steven Bane. "Physicochemical stability of the bevacizumab biosimilar, ABP 215, after preparation and storage in intravenous bags." Generics and Biosimilars Initiative Journal 9, no. 4 (December 15, 2020): 155–62. http://dx.doi.org/10.5639/gabij.2020.0904.026.
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Study Objectives: To evaluate extended in-use stability of bevacizumab biosimilar, ABP 215, after dilution into intravenous bags, extended storage, and simulated infusion to enable advanced preparation and storage. Methods: Two lots of ABP 215 were diluted to high- (16.5 mg/mL) and low- (1.4 mg/mL) dose concentrations in two types of intravenous bag under ambient light conditions. Dosed intravenous bags were stored at 2°C–8°C for 35 days, followed by 30°C for 2 days, and each bag was infused on Day 37. Analysis of purity and physicochemical stability was performed using size-exclusion high-performance liquid chromatography (SE-HPLC), cation-exchange high-performance liquid chromatography (CEX-HPLC), reduced capillary electrophoresis-sodium dodecyl sulphate (rCE-SDS), subvisible particle detection assays, visual inspection, and by measuring protein concentration and potency. Results: No meaningful changes were seen in ABP 215 purity when analysed by SE-HPLC, CEX-HPLC and rCE-SDS following dilution, storage and infusion of two lots, bags, and doses. Protein concentration remained consistent throughout the study for all samples and no significant loss in potency was detected. No potentially proteinaceous particles or increases in subvisible particles were observed. Discussion: This study investigated the in-use stability of ABP 215 following dilution, extended storage, and infusion, that represent worst-case handling conditions. ABP 215 exhibited consistent product quality and activity, with no significant degradation observed under the conditions tested. Conclusion: ABP 215 retains physicochemical stability after dilution over the recommended dosing concentrations, extended storage, and simulated infusion. This supports the advance preparation and storage of ABP 215 in intravenous bags for infusion.