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Khan, Mohammad Sharif, Jannatul Azmir, Ademario Iris da Silva Junior, Yong Foo Wong, Mamun Mollah, Jalal T. Althakafy, and Md Zaidul Islam Sarker. "Strategy for Sustainable and Green Chromatographic Separation Science: Innovation, Technology and Application." Current Chromatography 7, no. 1 (November 26, 2020): 5–16. http://dx.doi.org/10.2174/2213240607999200813195405.
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Green separation science involves extraction, pre-concentration and chromatographic analysis aiming at minimizing environmental impact by reducing energy and reagent usage and reducing or eliminating waste generation. However, the enrichment of trace analytes and/or the analysis of complex matrices most frequently require several steps before analysis, such as extraction, pre-concentration, clean up and preparative chromatography. Thus, alternative and greener separation techniques and solvents are replacing classical methods to diminish the carbon footprint and increase sustainability. Moreover, many innovations are also emerging to curtail the environmental impact of samples analysis; such as micro or nano analytical platforms, sensor-based systems and direct injection to high-resolution mass spectrometry. The current review provides an updated account of the green and sustainable separation science techniques. The current innovations on greener separations and their application in different fields of study are discussed.
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Memon, Najma, Tahira Qureshi, Muhammad Iqbal Bhanger, and Muhammad Imran Malik. "Recent Trends in Fast Liquid Chromatography for Pharmaceutical Analysis." Current Analytical Chemistry 15, no. 4 (July 3, 2019): 349–72. http://dx.doi.org/10.2174/1573411014666180912125155.
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Background: Liquid chromatography is the workhorse of analytical laboratories of pharmaceutical companies for analysis of bulk drug materials, intermediates, drug products, impurities and degradation products. This efficient technique is impeded by its long and tedious analysis procedures. Continuous efforts of scientists to reduce the analysis time resulted in the development of three different approaches namely, HTLC, chromatography using monolithic columns and UHPLC. Methods: Modern column technology and advances in chromatographic stationary phase including silica-based monolithic columns and reduction in particle and column size (UHPLC) have not only revolutionized the separation power of chromatographic analysis but also have remarkably reduced the analysis time. Automated ultra high-performance chromatographic systems equipped with state-ofthe- art software and detection systems have now spawned a new field of analysis, termed as Fast Liquid Chromatography (FLC). The chromatographic approaches that can be included in FLC are hightemperature liquid chromatography, chromatography using monolithic column, and ultrahigh performance liquid chromatography. Results: This review summarizes the progress of FLC in pharmaceutical analysis during the period from year 2008 to 2017 focusing on detecting pharmaceutical drugs in various matrices, characterizing active compounds of natural products, and drug metabolites. High temperature, change in the mobile phase, use of monolithic columns, new non-porous, semi-porous and fully porous reduced particle size of/less than 3μm packed columns technology with high-pressure pumps have been extensively studied and successively applied to real samples. These factors revolutionized the fast high-performance separations. Conclusion: Taking into account the recent development in fast liquid chromatography approaches, future trends can be clearly predicated. UHPLC must be the most popular approach followed by the use of monolithic columns. Use of high temperatures during analysis is not a feasible approach especially for pharmaceutical analysis due to thermosensitive nature of analytes.
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Durai Ananda Kumar T, Sai Charan, Venkateswarlu A, and Supriya Reddy K. "Evolution of liquid chromatography: Technologies and applications." International Journal of Research in Pharmaceutical Sciences 11, no. 3 (July 8, 2020): 3204–11. http://dx.doi.org/10.26452/ijrps.v11i3.2449.
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Liquid chromatographic offers efficient analyte separation employing high pressure pumps. The reversed phase high performance liquid chromatography (RP-HPLC) is widely utilized in the purity testing and quantitative determination of pharmaceuticals and neutraceuticals. The limitations of traditional liquid chromatography such as particle size, resolution and selectivity demanded for the developments and Waters Corporation developed ultraperformance liquid chromatography (UPLC). Ultrafast liquid chromatography (UFLC) is another milestone, which offers faster and efficient separation. Multidimensional UHPLC provides separation of complex molecules. The particle size decrease enhances the resolution of LC separation. Ethylene bridged hybrid (BEH), Charged surface hybrid (CSH) and Peptide separation technology (PST) offer better performance in. The amalgamation of chromatographic and spectroscopic detectors namely fluorescence detector (FD) and mass spectrometry (MS) provides efficient separation. Liquid chromatography (LC) offers the analysis of pharmaceuticals, biological, food materials, and natural products. This review covers technologies and recent pharmaceutical and biomedical applications of liquid chromatography technologies
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Xie, Chao Fan, Rey Chue Huang, Lin Xu, Fu Quan Zhang, and Lu Xiong Xu. "Digitized Simulation of the Moving Bed." Materials Science Forum 987 (April 2020): 157–61. http://dx.doi.org/10.4028/www.scientific.net/msf.987.157.
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Chromatographic separation is an indispensable and important technology in the manufacturing process of chemical products and biomedicine. It uses the distribution differences of a compound in the stationary phase and mobile phase to achieve the separation of the mixture. It is of great value to study the separation process of substances by simulated moving bed chromatography. By digitally simulating the process of moving bed, we can observe the influence of parameter changes on substance analysis by chromatography, and then find out the law of substance separation, which can provide theoretical basis for scientific research of biopharmaceuticals.
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Cong, Jing Xiang, Shao Yan Wang, and Hong Gao. "Separation of Liquiritin by Two-Dimensional Liquid Chromatography." Advanced Materials Research 455-456 (January 2012): 1232–38. http://dx.doi.org/10.4028/www.scientific.net/amr.455-456.1232.
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Two-dimensional liquid chromatography (2DLC) is an important technology for the separation and analysis of complex samples. Liquiritin, an important active component in licorice, was chosen as the target compound and it was separated by three kinds of off-line 2DLC, i.e. size exclusion chromatography × reversed phase chromatography, normal phase × reversed phase chromatography and reversed phase chromatography × reversed phase chromatography (SEC×RP, NP×RP and RP×RP). The chromatographic conditions were selected and the 2D systems were combined. The results show that it is feasible to separate Liquiritin from licorice extract using 2DLC. Among the 2D modes mentioned above, the highest purity of Liquiritin was obtained in the RP×RP mode, and the concentration of Liquiritin was increased most significantly in the NP×RP mode.
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Saad, Martin N., Hebatallah M. Essam, Eman S. Elzanfaly, and Sawsan M. Amer. "A Two-Step Optimization Approach: Validated RP-HPLC Method for Determination of Gatifloxacin and Dexamethasone in Ophthalmic Formulation." Journal of Chromatographic Science 58, no. 6 (April 13, 2020): 504–10. http://dx.doi.org/10.1093/chromsci/bmaa013.
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Abstract The growing technology of stationary phase chemistry has a great impact on the chromatographic system performance and analysis economics. In this context, a simple rapid reversed phase high-performance liquid chromatography method development is presented for the analysis of gatifloxacin (GFN) and dexamethasone sodium phosphate (DSP) in their ophthalmic formulation. A two-step optimization approach has been conducted using optimum chromatographic conditions as well as proper selection of stationary phase. The chromatographic separation was carried out using sodium phosphate buffer pH 3.0 ± 0.1 and acetonitrile 72:28 v/v, respectively, with flow rate 1 mL min−1 and simultaneous detection at 243 nm. Three different column technologies were investigated at the optimum set of the chromatographic conditions: Xbridge® bridged ethylene hybrid silica, Kinetex™ Core-Shell and the Onyx™ Monolithic stationary phase. The monolithic column has shown better chromatographic separation, based on system suitability testing as well as shorter analysis time and sensitivity. The proposed method was validated according to International Conference on Harmonization guidelines. The linearity was achieved for GFN and DSP in the range 0.58–120 μg mL−1 and 0.50–120 μg mL−1, respectively, with acceptable accuracy, precision and selectivity.
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Regal, Patricia, Mónica Díaz-Bao, Rocío Barreiro, Alberto Cepeda, and Cristina Fente. "Application of molecularly imprinted polymers in food analysis: clean-up and chromatographic improvements." Open Chemistry 10, no. 3 (June 1, 2012): 766–84. http://dx.doi.org/10.2478/s11532-012-0016-3.
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AbstractSeveral natural and synthetic substances have been monitored in analytical laboratories worldwide to ensure food safety. Multiple residue detection (i.e., detection of multiple analytes in a single sample or matrix) is a main weakness of existing analytical methods, when fast and reliable results are required. Multianalyte approaches may save time and money in the food industry, and more importantly, they allow the quick release of food products into the marketplace. In addition, multianalyte approaches notably decrease the time required between sampling and analysis to meet legal requirements. However, to achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. In addition, good chromatographic separation methods are also necessary to distinguish closely related analytes. Molecular imprinting technology (MIT) is an emerging, powerful tool for sample extraction and chromatography. First used for solid-phase extraction, molecularly imprinted polymers (MIPs) are also effective chromatographic phases for the separation of isomers and structurally related molecules. In recent years, a number of analytical methods utilising MIT have been applied for the analysis of residues in food, and existing methodologies have been improved. This review article describes the latest applications of MIT in the development of methodologies to monitor the presence of residues of veterinary products in foodstuff.
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Peace, Robert W., and G. Sarwar Gilani. "Chromatographic Determination of Amino Acids in Foods." Journal of AOAC INTERNATIONAL 88, no. 3 (May 1, 2005): 877–87. http://dx.doi.org/10.1093/jaoac/88.3.877.
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Abstract Amino acids in foods exist in a free form or bound in peptides, proteins, or nonpeptide bonded polymers. Naturally occurring L-amino acids are required for protein synthesis and are precursors for essential molecules, such as co-enzymes and nucleic acids. Nonprotein amino acids may also occur in animal tissues as metabolic intermediates or have other important functions. The development of bacterially derived food proteins, genetically modified foods, and new methods of food processing; the production of amino acids for food fortification; and the introduction of new plant food sources have meant that protein amino acids and amino acid enantiomers in foods can have both nutritional and safety implications for humans. There is, therefore, a need for the rapid and accurate determination of amino acids in foods. Determination of the total amino acid content of foods requires protein hydrolysis by various means that must take into account variations in stability of individual amino acids and resistance of different peptide bonds to the hydrolysis procedures. Modern methods for separation and quantitation of free amino acids either before or after protein hydrolysis include ion exchange chromatography, high performance liquid chromatography (LC), gas chromatography, and capillary electrophoresis. Chemical derivatization of amino acids may be required to change them into forms amenable to separation by the various chromatographic methods or to create derivatives with properties, such as fluorescence, that improve their detection. Official methods for hydrolysis and analysis of amino acids in foods for nutritional purposes have been established. LC is currently the most widely used analytical technique, although there is a need for collaborative testing of methods available. Newer developments in chromatographic methodology and detector technology have reduced sample and reagent requirements and improved identification, resolution, and sensitivity of amino acid analyses of food samples.
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Mazurova, K. M., M. S. Tyutlikova, E. A. Chudin, A. V. Domovenko, A. A. Makarov, A. L. Pakhomov, and V. A. Vinokurov. "Increasing the Efficiency and Selectivity of Separation of Components in Chromatographic Analysis of Natural Gas." Chemistry and Technology of Fuels and Oils 56, no. 6 (January 2021): 909–18. http://dx.doi.org/10.1007/s10553-021-01207-0.
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Dwyer, James L., and Ming Zhou. "Polymer Characterization by Combined Chromatography-Infrared Spectroscopy." International Journal of Spectroscopy 2011 (December 18, 2011): 1–13. http://dx.doi.org/10.1155/2011/694645.
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Infrared spectroscopy is widely used in the analysis and characterization of polymers. Polymer products are not a singular species, but rather, they are a population of polymer molecules varying in composition and configuration plus other added components. This paper describes instrumentation that provides the benefit or resolving polymer populations into discrete identifiable entities, by combining chromatographic separation with continuous spectra acquisition. The technology also provides a way to determine the mass distribution of discrete components across the chromatographic distribution of a sample. Various examples of application of this technology to polymer products are described. Examples include additives analysis, resolution of polymer blends, composition characterization of copolymers, analysis of degradation byproducts, and techniques of analysis of reactive polymer systems.
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Onuska, Francis I., Ken A. Terry, and R. James Maguire. "Analysis of Aromatic Amines in Industrial Wastewater by Capillary Gas Chromatography-Mass Spectrometry." Water Quality Research Journal 35, no. 2 (May 1, 2000): 245–62. http://dx.doi.org/10.2166/wqrj.2000.016.
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Abstract The analysis of aromatic amines, particularly benzidines, at trace levels in environmental media has been difficult because of the lack of suitable deactivated capillary column stationary phases for gas chromatography. This report describes the use of an improved type of column as well as a method for the analysis of anilines and benzidines in water, wastewater and sewage samples. Extraction procedures are applicable to a wide range of compounds that are effectively partitioned from an aqueous matrix into methylene chloride, or onto a solid-phase extraction cartridge. The extracted analytes are also amenable to separation on a capillary gas chromatographic column and transferable to the mass spectrometer. These contaminants are converted to their N-trifluoroacetyl derivatives. Aniline and some substituted anilines, and 3,3’-dichlorobenzidine and benzidine were determined in 24-h composite industrial water, wastewater, primary sludge and final effluent samples at concentrations from 0.03 up to 2760 µg/L.
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Fischer, Jenny J., Olivia Graebner, Mathias Dreger, Mirko Glinski, Sabine Baumgart, and Hubert Koester. "Improvement of Capture Compound Mass Spectrometry Technology (CCMS) for the Profiling of Human Kinases by Combination with 2D LC-MS/MS." Journal of Biomedicine and Biotechnology 2011 (2011): 1–5. http://dx.doi.org/10.1155/2011/850589.
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An increasingly popular and promising field in functional proteomics is the isolation of proteome subsets based on small molecule-protein interactions. One platform approach in this field are Capture Compounds that contain a small molecule of interest to bind target proteins, a photo-activatable reactivity function to covalently trap bound proteins, and a sorting function to isolate captured protein conjugates from complex biological samples for direct protein identification by liquid chromatography/mass spectrometry (nLC-MS/MS). In this study we used staurosporine as a selectivity group for analysis in HepG2 cells derived from human liver. In the present study, we combined the functional isolation of kinases with different separation workflows of automated split-free nanoflow liquid chromatography prior to mass spectrometric analysis. Two different CCMS setups, CCMS technology combined with 1D LC-MS and 2D LC-MS, were compared regarding the total number of kinase identifications. By extending the chromatographic separation of the tryptic digested captured proteins from 1D LC linear gradients to 2D LC we were able to identify 97 kinases. This result is similar to the 1D LC setup we previously reported but this time 4 times less input material was needed. This makes CCMS of kinases an even more powerful tool for the proteomic profiling of this important protein family.
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Harnly, James M., Devanand Luthria, and Pei Chen. "Detection of Adulterated Ginkgo biloba Supplements Using Chromatographic and Spectral Fingerprints." Journal of AOAC INTERNATIONAL 95, no. 6 (November 1, 2012): 1579–87. http://dx.doi.org/10.5740/jaoacint.12-096.
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Abstract The fingerprints of 18 commercially available Ginkgo biloba supplements, 12 samples of raw G. biloba leaves, and three G. biloba standard reference materials from the National Institute of Standards and Technology were acquired directly (no chromatography) by UV spectrometry and after separation using HPLC with a diode array detector. The fingerprints consisted of the UV spectral images, the chromatographic images, and the areas of the 21 most prominent chromatographic peaks. Data were analyzed by principal component analysis and one-class soft independent modeling of class analogy (SIMCA). It was determined that three of the commercial products were adulterated with rutin, four with quercetin, and one with an unidentified flavonol glycoside. One-class SIMCA of the authentic products allowed the adulterated products to be easily distinguished using Q-residuals. Authentic supplements and raw leaf materials were easily distinguished. The finely powdered samples were also analyzed by near-IR (NIR) spectrometry. The authentic and adulterated products could not be distinguished by NIR spectrometry because of the excipients.
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Kurbanoglu, Sevinc, Ozer Karsavurdan, and Sibel A. Ozkan. "Recent Advances on Drug Analyses Using Ultra Performance Liquid Chromatographic Techniques and their Application to the Biological Samples." Current Analytical Chemistry 15, no. 3 (May 7, 2019): 277–93. http://dx.doi.org/10.2174/1573411014666180423152612.
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Introduction: Ultra-Performance Liquid Chromatographic (UPLC) method enables analyst to establish an analysis at higher pressure than High Performance Liquid Chromatographic (HPLC) method towards liquid chromatographic methods. UPLC method provides the opportunity to study a higher pressure compared to HPLC, and therefore smaller column in terms of particle size and internal diameter are generally used in drug analysis. The UPLC method has attracted gradually due to its advantages such as short analysis time, the small amount of waste reagents and the significant savings in the cost of their destruction process. In this review, the recent selected studies related to the UPLC method and its method validation are summarized. The drug analyses and the results of the studies which were investigated by UPLC method, with certain parameters from literature are presented. Background: Quantitative determination of drug active substances by High-Performance Liquid Chromatography (HPLC) from Liquid Chromatography (LC) methods has been carried out since the 1970's with the use of standard analytical LC methods. In today's conditions, rapid and very fast even ultra-fast, flow rates are achieved compared to conventional HPLC due to shortening analysis times, increasing method efficiency and resolution, reducing sample volume (and hence injection volume), reducing waste mobile phase. Using smaller particles, the speed and peak capacity are expanding to new limit and this technology is named as Ultra Performance Liquid Chromatography. In recent years, as a general trend in liquid chromatography, ultra-performance liquid chromatography has taken the place of HPLC methods. The time of analysis was for several minutes, now with a total analysis time of around 1-2 minutes. The benefits of transferring HPLC to UPLC are much better understood when considering the thousands of analyzes performed for each active substance, in order to reduce the cost of analytical laboratories where relevant analysis of drug active substances are performed without lowering the cost of research and development activities. Methods: The German Chemist Friedrich Ferdinand Runge, proposed the use of reactive impregnated filter paper for the identification of dyestuffs in 1855 and at that time the first chromatographic method in which a liquid mobile phase was used, was reviewed. Christian Friedrich Chönbein, who reported that the substances were dragged at different speeds in the filter paper due to capillary effect, was followed by the Russian botanist Mikhail S. Tswet, who planted studies on color pigment in 1906. Tswet observes the color separations of many plant pigments, such as chlorophyll and xanthophyll when he passes the plant pigment extract isolated from plant through the powder CaCO3 that he filled in the glass column. This method based on color separation gives the name of "chromatographie" chromatography by using the words "chroma" meaning "Latin" and "graphein" meaning writing. Results and Conclusion: Because the UPLC method can be run smoothly at higher pressures than the HPLC method, it offers the possibility of analyzing using much smaller column sizes and column diameters. Moreover, UPLC method has advantages, such as short analysis time, the small amount of waste reagents and the significant savings in the cost of their destruction process. The use of the UPLC method especially analyses in biological samples such as human plasma, brain sample, rat plasma, etc. increasingly time-consuming due to the fact that the analysis time is very short compared to the HPLC, because of the small amount of waste analytes and the considerable savings in their cost.
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Maris, Christophe, Alain Laplanche, Jean Morvan, and Marianne Bloquel. "Development of a Packed Precolumn for Capillary Gas Chromatographic Analysis of Amines in Acidic Aqueous Solution." Water Science and Technology 40, no. 6 (September 1, 1999): 141–48. http://dx.doi.org/10.2166/wst.1999.0283.
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This paper describes an optimization of the analysis of amines in aqueous solution. Direct injection of the acidic sample (HCl 0.12 N) is performed by the coupling of packed precolumn with a capillary column. The basic support efficiently traps residual vapors of hydrochloric acid and water at the injection time; the capillary chromatographic performance is maintained. The precolumn coupling with PoraPLOT Amines capillary column enables a separation and quantification of the lower volatile aliphatic amines (methylamine, dimethylamine, trimethylamine and ethylamine). The ammonia addition to the solution (200 ppm NH3) reduces amine adsorption in the column. The analysis repeatability is about 5% for a 50μM amine mixture and 21% for the quantification limit of 0.5 μM with a sensitive and specific nitrogen phosphor detector. The precolumn avoids using split injection (sensitivity increased). Other nitrogen compounds can be analyzed by this system: aromatic amines (aniline) and unsaturated nitrogen heterocycles (pyridine). This new technique increases the chromatographic performances in comparison with usual methods; its automation is possible.
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Salama, Nahla N., and Shudong Wang. "Quantitative Mass Spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation." Analytical Chemistry Insights 4 (January 2009): ACI.S2564. http://dx.doi.org/10.4137/aci.s2564.
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The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL−1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%-102.75% was obtained. The method is accurate (% RE <; 5%) and reproducible with intra- and inter-assay precision (RSD% <; 8.0%). The quantification limit is 23.8 ng mL−1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.
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Seo, Chang-Seob, and Mee-Young Lee. "Simultaneous Analysis to Evaluate the Quality of Insamyangpye–Tang Using High-Performance Liquid Chromatography–Photo Diode Array Detection." Applied Sciences 11, no. 11 (May 24, 2021): 4819. http://dx.doi.org/10.3390/app11114819.
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Insamyangpye–tang (ISYPT) is a traditional medicinal formula comprised of 13 herbs and has been used in East Asia to treat lung-related diseases. However, to our knowledge, no method of analysis for its quality control has been reported. In this study, a method of analysis for quality control of ISYPT was developed using high-performance liquid chromatography. Chromatographic separation, analysis, and assay verification were performed with a distilled water–acetonitrile mobile phase system, both containing 0.1% (v/v) trifluoroacetic acid, and a Gemini C18 analytical column (4.6 mm × 250 mm, 5 μm) using authentic standards for eight marker compounds. These marker constituents were detected simultaneously at 0.09–5.95 mg/g. The analysis method developed can be used for basic quality control of ISYPT.
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Sun, Rong, Chengran Hu, Qian Dou, and Libiao Luan. "Simultaneous Determination of Nine Residual Solvents in Sorafenib Tosylate by Gas Chromatography." Journal of AOAC INTERNATIONAL 104, no. 4 (March 23, 2021): 1005–9. http://dx.doi.org/10.1093/jaoacint/qsab041.
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Abstract Background Direct injection gas chromatography is convenient and quick. The residual solvent with a higher boiling point can be measured by using direct inhection gas chromatography. This method could be developed for residual solvents analysis of sorafenible tosylate. Objective In the present investigation, the injection method was developed and validated for the detection and quantification of residual solvents in sorafenib tosylate. Method The nine kinds of residual solvents were separated using direct injection gas chromatographic technology, and a quantitative analysis was performed. Analytical performance of the proposed injection method was validated as per the defined guidelines with respect to linearity, accuracy, precision, robustness, and specificity. Results Under the optimized conditions, simultaneous separation and determination of nine kinds of residual solvents, including methanol, acetonitrile, ethyl acetate, tetrahydrofuran, chlorobenzene, toluene, acetone, dichloromethane, and N, N-dimethylformamide were carried out using a DB-WAXETR polyethylene glycol Inertap Pure-WAX column (30 m × 0. 32 mm × 0.25 µm) for separation. The calibration plot was found to be linear, accurate, precise, robust, and specific for direct injection gas chromatography. The residual solvents in sorafenib tosylate were quantified by the developed method. Conclusions The present method was successfully applied for analysis of residual solvents in sorafenib tosylate. Similarly, the method can be used for quality control and stability testing of other medicines. Highlights A validated GC assay for the combined analysis of the nine solutions which offered a reference method for the detection of residual solvents in other medicines.
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Fathi, Haghighe, Robab Soltani-Jigheh, and Saeed Hemmati. "Using nanometer TiO2 modified with cetyl trimethyl ammonium bromide for separation and preconcentration of Parathion in water sample." Water Supply 17, no. 2 (August 23, 2016): 362–71. http://dx.doi.org/10.2166/ws.2016.140.
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In this work, nanometer TiO2 modified by cetyl trimethyl ammonium bromide (CTAB) was used as adsorbent for solid-phase extraction (SPE) of Parathion in environmental water samples. Adsorbed Parathion was then desorbed with different eluents and determined by gas chromatography (GC)/flame ionization detection. Greater selectivity, resolution, and sensitivity have been seen by GC compared with other methods. Parameters that might influence the extraction efficiency, such as the eluent type and its volume, adsorbent amount, sample volume, sample pH and sample flow rate, were optimized. Under the optimized extraction conditions with toluene as the eluent, the experimental results showed the excellent linearity of Parathion (R2 > 0.99) over the range of 0.01–0.8 μg/mL, and the relative standard deviation was 6.3% (n = 5). The detection limit of the proposed method could reach 0.024 ng/mL based on the ratio of chromatographic signal to base line noise (S/N = 3). Recovery of 93% was achieved with spiked water samples. The method was successfully applied to the analysis of surface water samples.
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Chang, L. W., E. Atlas, and C. S. Giam. "Chromatographic Separation and Analysis of Chlorinated Hydrocarbons and Phthalic Acid Esters from Ambient Air Samples." International Journal of Environmental Analytical Chemistry 19, no. 2 (January 1985): 145–53. http://dx.doi.org/10.1080/03067318508077024.
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Nuzzo, Genoveffa, Emiliano Manzo, Marcello Ziaco, Laura Fioretto, Ana Margarida Campos, Carmela Gallo, Giuliana d’Ippolito, and Angelo Fontana. "UHPLC-MS Method for the Analysis of the Molecular Adjuvant Sulfavant A." Applied Sciences 11, no. 4 (February 5, 2021): 1451. http://dx.doi.org/10.3390/app11041451.
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A fast and sensitive method that is based on Ultra High Performance Liquid Chromatography coupled with High Resolution Mass Spectrometry (UHPLC-HRMS) for the measurement of Sulfavant A, a molecular adjuvant with a sulfolipid skeleton, is described. The method has been validated over the linearity range of 2.5–2000 ngmL−1 using a deuterated derivative (d70-Sulfavant A) as internal standard. Chromatographic separation is based on a UHPLC Kinetex® 2.6 µm PS C18 column and a gradient of methanol in 0.32 mM ammonium hydroxide solution buffered at pH 8. The lowest limit of quantification of Sulfavant A was 6.5 ngmL−1. The analytical procedure was tested on an extract of mice lung spiked with 30, 300, and 1500 ng of Sulfavant A. The analysis revealed a precision and accuracy value (as a mean value of all the quality control samples analyzed) of 4.7% and 96% in MeOH and 6.4% and 93.4% in the lung extracts, respectively.
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Farrar-Khan, J. R., G. E. Andrews, R. Ishaq, P. T. Williams, and K. D. Battle. "Quantitative Diesel Particulate Analysis Using Gas Chromatography/Mass Spectrometry." Proceedings of the Institution of Mechanical Engineers, Part A: Journal of Power and Energy 207, no. 2 (May 1993): 95–106. http://dx.doi.org/10.1243/pime_proc_1993_207_018_02.
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Detailed analysis of the composition of diesel particulate solvent organic fraction (SOF) is difficult for low-level polycyclic aromatic hydrocarbons (PAH) and generally requires pre-separation of aromatic and aliphatic compounds. This is usually done using either on-line or off-line high performance liquid chromatography (HPLC) which complicates the SOF analysis. Without pre-separation of the samples the gas chromatography (GC) cannot resolve the low-level PAH in the presence of higher levels of n-alkanes and other compounds, which may co-elute. A Finnegan Mat ion trap mass spectrometry (MS) detector was used with a Carlo Erba Mega GC to analyse diesel fuel, diesel particulate SOF and oil without pre-separation. It was shown that the mass number of PAH could easily be extracted from the total ion chromatogram and low-level PAH quantified without pre-separation. A standard calibration mix of PAH covering the mass range of interest was used and the computer software developed to search for and quantify them automatically. This calibration mixture could also be used for the quantification of any other PAH. Pre-separation of the SOF was only necessary for very low-level PA H in the ppb range.
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Midttun, Ø., and O. M. Kvalheim. "Interactions in chromatographic separation of resins from deasphaltened crude oils studied by means of infrared spectroscopy and principal component analysis." Fuel 80, no. 5 (April 2001): 717–30. http://dx.doi.org/10.1016/s0016-2361(00)00147-2.
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Wu, Manli, Huining Xu, Ya Yu, and Lili Wang. "High performance liquid chromatography–tandem mass spectrometry for rapid and sensitive analysis of six polycyclic aromatic hydrocarbons in wastewater." Water Science and Technology 64, no. 2 (July 1, 2011): 477–84. http://dx.doi.org/10.2166/wst.2011.710.
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A sensitive and fast method was developed to quantitatively analyse the six polycyclic aromatic hydrocarbons (fluoranthene (FLT), benzo[b]fluoranthene (BbF), benzo[k]fluoranthene (BkF), benzo[a]pyrene (Bap), benzo[ghi]perylene (BghiP) and indeno[1,2,3-cd]pyrene (INPY)) by high performance liquid chromatography (UPLC) coupling with tandem mass spectrometry (MS/MS). Chromatographic separation was performed on a Waters Acquity UPLCTM BEHC18 column (1.7 μm, 2.1 mm × 50 mm). A 0.2 μm precolumn filter was used to protect the analytical column. Mobile phase A was acetonitrile containing 0.5% toluene. Mobile phase B was water. Linearity of detection was in the range of 1–100 μg L−1; LOD of 5 PAHs were lower than 0.1 μg L−1; LOQ were 0.2 μg L−1 except for benzo[k]fluoranthene. The LOD and the LOQ of benzo[k]fluoranthene were respectively 0.1 μg L−1 and 0.8 μg L−1. Wastewater samples collected from two wastewater treatment plants were determined using this method respectively. Recovery of all compounds varied from 67.8 ± 10.6% to 113.2 ± 7.2%. In comparison with the existing methods, this rapid method saves time and solvent and improves instrument sample throughput by 2–5 fold.
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Parys, Wioletta, Małgorzata Dołowy, and Alina Pyka-Pająk. "Current Strategies for Studying the Natural and Synthetic Bioactive Compounds in Food by Chromatographic Separation Techniques." Processes 9, no. 7 (June 24, 2021): 1100. http://dx.doi.org/10.3390/pr9071100.
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The present study summarizes the new strategies including advanced equipment and validation parameters of liquid and gas chromatography methods i.e., thin-layer chromatography (TLC), column liquid chromatography (CLC), and gas chromatography (GC) suitable for the identification and quantitative determination of different natural and synthetic bioactive compounds present in food and food products, which play an important role in human health, within the period of 2019–2021 (January). Full characteristic of some of these procedures with their validation parameters is discussed in this work. The present review confirms the vital role of HPLC methodology in combination with different detection modes i.e., HPLC-UV, HPLC-DAD, HPLC-MS, and HPLC-MS/MS for the determination of natural and synthetic bioactive molecules for different purposes i.e., to characterize the chemical composition of food as well as in the multi-residue analysis of pesticides, NSAIDs, antibiotics, steroids, and others in food and food products.
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Jo, Hyeong-Wook, Min-Goo Park, Hwang-Ju Jeon, Joon-Kwan Moon, and Sung-Eun Lee. "Analysis of Multiresidue Pesticides in Agricultural Paddy Soils Near Industrial Areas in Korea by GC–MS/MS and LC–MS/MS Using QuEChERS Extraction with dSPE Clean-Up." Applied Sciences 11, no. 18 (September 10, 2021): 8415. http://dx.doi.org/10.3390/app11188415.
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Pesticides have been used to control pests in agricultural fields and storage systems before circulating agricultural products to markets. A tandem mass spectrometry, equipped with gas chromatographic separation (GC–MS/MS) or ultra-performance liquid chromatographic separation (LC–MS/MS), was used to monitor residual pesticides in Korean rice paddy soils. Selective multiple reaction monitoring was employed during the analyses to achieve multiresidue pesticide analysis using GC–MS/MS and LC–MS/MS of 342 pesticides. In this study, QuEChERS extraction was employed with a dSPE clean-up to establish an effective pretreatment process. The limit of detection (LOD) and limit of quantification (LOQ) were set up for all pesticides, and method validation was performed for linearity and recovery at levels of 10 and 50 mg kg−1 in the untreated soil sample. All pesticides satisfied the acceptable recovery range of 70–120%, within less than 20% RSD values, except for ametoctradin and gibberellic acid. In the paddy soil analyses, tricyclazole was the most frequently detectable pesticide, followed by oxadiazon, endosulfan, and chlorantraniliprole. Continuous monitoring of residual pesticides in paddy soils should be conducted due to the translocation of some systemic pesticides from soils to crop plants, and the impact of residual pesticides on the environment.
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Brezovska, Katerina, Gabriela Petrovska, Jelena Acevska, Natalija Nakov, Ana Poceva-Panovska, Jasmina Tonic-Ribarska, Maja Hadzieva, and Aneta Dimitrovska. "Transfer of pharmacopoeial liquid chromatography reversedphase methods for determination of related compounds in diclofenac sodium and metamizole sodium from conventional to core-shell column." Macedonian Pharmaceutical Bulletin 61, no. 01 (2015): 13–18. http://dx.doi.org/10.33320/maced.pharm.bull.2015.61.01.003.
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Core-shell silica particles were developed as a new material for chromatographic stationary phases in order to provide fast and high efficiency separations of small and large molecules and complex samples, at pressures compatible with conventional HPLC equipment. The aim of our work was to show the applicability of the HPLC columns based on a core-shell technology for determination of related substances in diclofenac sodium and in metamizole sodium using the methods described in the corresponding monographs of the European pharmacopoeia. The obtained results have shown that the proposed methods can be successfully transferred on core shell column, with suitable adjustment of injection volume and flow rate. The advantage of using core-shell column is fast and highly efficient separation on conventional HPLC equipment with increased sensitivity of the method and high throughput of the analysis, providing enhanced lab productivity and reduced costs.
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Sato, Masaki, Motonobu Goto, Akio Kodama, and Tsutomu Hirose. "Chromatographic Analysis of Limonene and Linalool on Silica Gel in Supercritical Carbon Dioxide." Separation Science and Technology 33, no. 9 (January 1998): 1283–301. http://dx.doi.org/10.1080/01496399808544984.
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Hefnawy, Mohamed M., Maha A. Sultan, and Mona M. Al-Shehri. "Direct Enantiomeric Resolution of Betaxolol with Application to Analysis of Pharmaceutical Products." Analytical Chemistry Insights 1 (January 2006): 117739010600100. http://dx.doi.org/10.1177/117739010600100003.
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A high-performance liquid chromatographic (HPLC) method has been developed for the separation and determination of S- and R-enantiomers of betaxolol in tablets and ophthalmic preparations. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with fluorescence detection at excitation/emission wavelengths 275/305 nm. The polar ionic mobile phase (PIM) consists of methanol-glacial acetic acid-triethylamine, (100:0.020:0.025, v/v/v) has been used at a flow rate of 1.5 ml/min. All analytes with S-(-)-atenolol as internal standard were conducted at ambient temperature. The method is highly specific where another coformulated compounds did not interfere. The stability of betaxolol enantiomers under different degree of temperature also studied. The results showed that it is stable for at least 7 days at 70°C. The method validated for its linearity, accuracy, precision and robustness. Experimental design was used during validation to evaluate method robustness. Using the chromatographic conditions described, S- and R-betaxolol were well resolved with mean retention times of 11.3 and 12.6 min, respectively. Linear response (r > 0.997) was observed over the range of 10-500 ng/ml of betaxolol enantiomers, with detection limit of 5 ng/ml. The recoveries of S- and R-betaxolol from tablets and ophthalmic preparation ranged from 97.4 to 101.4% and 98.0 to 102.0%, respectively. The mean relative standard deviation (R.S.D.%) for both enantiomers were 1.1-1.4% and 1.3-1.7% in tablets and ophthalmic solution, respectively.
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Linhares, Ana Luiza Freitas de Assis, and Mauricio Yonamine. "Analysis of biofluids by paper spray-MS in forensic toxicology." Bioanalysis 12, no. 15 (August 2020): 1087–102. http://dx.doi.org/10.4155/bio-2020-0160.
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Direct ambient ionization techniques have been developed with the aim to reduce the complexity of mass spectrometry analysis by minimizing sample preparation and chromatographic separation. In this context, paper spray-MS (PS-MS) is an innovative approach that provides faster and cheaper analysis of biofluids by the addition of the sample directly to a paper. In forensic toxicology, the analytical workflow for the detection and quantification of drugs of abuse is onerous, including sample treatment, extraction and clean up, especially regarding complex biological matrices. PS-MS allows the detection of analytes of toxicological interest in blood, plasma and urine using low sample volume. This review aims to discuss the potential use, advances and challenges of PS-MS in forensic toxicology.
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Hernandez-Baez, Diana M., Alastair Reid, Antonin Chapoy, Bahman Tohidi, and Roda Bounaceur. "Establishing the Maximum Carbon Number for Reliable Quantitative Gas Chromatographic Analysis of Heavy Ends Hydrocarbons. Part 2. Migration and Separation Gas Chromatography Modeling." Energy & Fuels 27, no. 4 (March 26, 2013): 2336–50. http://dx.doi.org/10.1021/ef302009n.
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Qin, Shili, Fenglong Jin, Lidi Gao, Liqiang Su, Yingjie Li, Shuang Han, and Peng Wang. "Determination of sulfamerazine in aquatic products by molecularly imprinted capillary electrochromatography." Royal Society Open Science 6, no. 6 (June 2019): 190119. http://dx.doi.org/10.1098/rsos.190119.
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A molecularly imprinted monolith was prepared and evaluated for the special selective separation of sulfamerazine (SMR) by capillary electrochromatography (CEC). The single-step in situ polymerization method was applied through thermally immobilized vinyl groups of itaconic acid and a derivatization capillary column using SMR as the template. The monolith with optimal selectivity and permeability was performed at 45°C for 7 h according to the molar ratios of 1 : 4 : 10 (template/functional monomer/cross-linker). Under the optimized separation conditions of 75% acetonitrile in 20 mM phosphate buffer with pH 5.0, 15 kV applied voltage and 20°C column temperature, the imprinted monolith showed strong recognition ability for SMR and high column performance. Finally, the molecularly imprinted monolith coupled with the CEC method was successfully developed for the quantification of SMR in aquatic products, which was properly validated by a good linear relationship, recoveries and limit of detection. The coupling technique of the molecularly imprinted technology and CEC achieved pre-treatment enrichment and separation analysis in only one miniaturized chromatographic column.
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Chew, H. K., S. Miyamoto, H. An, D. Rocke, and C. Lebrilla. "Serum glycan analysis in metastatic breast cancer." Journal of Clinical Oncology 25, no. 18_suppl (June 20, 2007): 11504. http://dx.doi.org/10.1200/jco.2007.25.18_suppl.11504.
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11504 Background: There is a need for a reliable breast cancer biomarker that can predict a patient’s response to therapy. Serum glycans, or oligosaccharides, are of particular interest as over half of all proteins are glycosylated and alterations in glycosylation influence growth, adhesion, metastasis and immune surveillance of tumor, among other important functions. Serum glycans can be analyzed by high resolution mass spectrometry. Methods: Sera from patients with known metastatic breast cancer and age-matched healthy controls without medical problems were prospectively analyzed by mass spectroscopy. Women over the age of 18, who were not pregnant or breastfeeding, and who were without other active cancers were eligible. Samples were de-identified for laboratory personnel who analyzed sera by matrix-assisted laser desoprtion/ionization (MALDI) and Fourier transform ion-cyclotron resonance mass sepctrometry (FT ICR MS). Glycans were also profiled by chromatographic separation using a microchip nanoLC (Agilent) with a time-of-flight (TOF) mass analyzers. Results: Sera from 25 patients with metastatic breast cancer and 25 controls were evaluated. The mass profiles were obtained corresponding to both N-linked oligosaccharides (N-glycans) and O-linked oligosaccharides (O-glycans). Distinct variations in glycosylation were observed among sera analyzed from patients with metastatic breast cancer compared to controls. Specific glycan masses were analyzed and found to correspond to N-glycans. The chromatographic glycan profile showed individual glycans that were distinct for the cancer patients. Conclusions: Analysis of serum gylcans by mass spectrometry represents a new paradigm of cancer biomarker studies, focusing on post-translational modifications of proteins, rather than protein expression. Further refinement of this technology may be clinically useful in monitoring response to therapy in metastatic breast cancer. No significant financial relationships to disclose.
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Kalikova, Lyubov Borisovna, and E. R. Boyko. "Determination of adenine nucleotides by the modified method of high-performance liquid chromatography." Russian Clinical Laboratory Diagnostics 66, no. 3 (March 30, 2021): 172–76. http://dx.doi.org/10.51620/0869-2084-2021-66-3-172-176.
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Adenine nucleotides (ATP, ADP and AMP) play a central role in the regulation of metabolism and energy: they provide the energy balance of the cell, determine its redox state, act as allosteric effectors of a number of enzymes, modulate signaling and transcription factors and activate oxidation or biosynthesis substrates. A large number of methods have been developed to determine the level of ATP, ADP and AMP, but the most universal and effective method for the separation and analysis of complex mixtures is the reversed-phase high-performance liquid chromatography method (RP-HPLC). The aim of this study is to determine the optimal conditions for the qualitative separation and quantitative determination of standard solutions of ATP (1 mmol/l), ADP (0,5 mmol/l) and AMP (0,1 mmol/l) by RP-HPLC. The degree of separation of adenine nucleotides was estimated by the time of peak output in the chromatogram. To achieve the goal, the following tasks were set: assess the effect of the temperature of the analysis on the separation and change of the release time of the analytes in the chromatogram; determine the most optimal composition of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram (the content of the organic solvent in the solution); to identify the effect of pH of the mobile phase on the separation of standard solutions of adenine nucleotides; set the optimal molarity of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram. It was found that the temperature of the analysis does not affect the quality of peak separation, while the composition and pH of the mobile phase have a significant effect on the complete and clear separation of the studied nucleotides in the chromatogram. It was determined that the analysis temperature of 37°C and the mobile phase of 0.05 M KH2PO4 (pH 6.0) are optimal for separating the peaks of adenine nucleotides.
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Onofrio, Michelle D., Claude R. Mallet, Allen R. Place, and Juliette L. Smith. "A Screening Tool for the Direct Analysis of Marine and Freshwater Phycotoxins in Organic SPATT Extracts from the Chesapeake Bay." Toxins 12, no. 5 (May 13, 2020): 322. http://dx.doi.org/10.3390/toxins12050322.
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Many detection methods for phycotoxins, bioactive compounds produced by harmful algae, focus on one compound or a class of related compounds. Multiple harmful algal species often co-occur in the environment, however, emphasizing the need to analyze for the presence of multiple groups of marine and freshwater phycotoxins in environmental samples, e.g., extracts from solid phase adsorption toxin tracking (SPATT). Two methods were developed to screen for 13 phycotoxins (microcystin-RR, -LR, -YR, azaspiracid-1, -2, karlotoxin 3, goniodomin A, brevetoxin-2, yessotoxin, pectenotoxin-2, dinophysistoxin-1, -2, and okadaic acid) in organic SPATT extracts using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) equipped with a trapping dimension (trap) and at-column dilution (ACD). The performance of each compound under 36 combinations of chromatographic conditions was characterized, and two final methods, acidic and basic, were selected based on peak shapes, signal intensities, resolution, and the separation in time of positive and negative MS ionization modes. Injection volumes of up to 1 mL were possible through trap/ACD technology, resulting in limits of detection between 0.001 and 0.05 µg/L across the analytes. Benefits highlighted in this study, beyond the improved detection limits and co-detection of multiple toxin groups, include the ability to inject samples of 100% organic solvent, ensuring analyte stability and streamlining workflow through the elimination of laborious sample preparation steps.
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Schobel, Uwe, Michel Frenay, Danny A. Van Elswijk, Joanne M. McAndrews, Kelly R. Long, Lisa M. Olson, Steven C. Bobzin, and Hubertus Irth. "High Resolution Screening of Plant Natural Product Extracts for Estrogen Receptor a and f3 Binding Activity Using an Online HPLC-MS Biochemical Detection System." Journal of Biomolecular Screening 6, no. 5 (October 2001): 291–303. http://dx.doi.org/10.1177/108705710100600503.
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A new screening technology that combines biochemical analysis with the resolution power of high-performance liquid chromatography (HPLC), referred to here as high-resolution screening (HRS) technique, is described. The capability of the HRS technology to analyze biologically active compounds in complex mixtures is demonstrated by screening a plant natural product extract library for estrogen receptor (ER) a and fi binding activity. The simultaneous structure elucidation of biologically active components in crude extracts was achieved by operating the HRS system in combination with mass spectrometry (MS). In contrast to conventional microtiter-type bioassays, the interactions of the extracts with the ER and the employed label, coumestrol, proceeded at high speed in a closed, continuous-flow reaction detection system, which was coupled directly to the outlet of a HPLC separation column. The reaction products of this homogeneous fluorescence enhancement-type assay were detected online using a flow-through fluorescence detector. Primary screening of the extract library was performed in the fast-flow injection analysis mode (FlowScreening) wherein the chromatographic separation system was bypassed. The library was screened at high speed, using two assay lines in parallel. A total of 98% of the identified hits were confirmed in a traditional 96-well microplate-based fluorescence polarization assay, indicating the reliability of the FlowScreening process. Active extracts were reassayed in a transcriptional activation assay in order to assess the functional activity of the bioactive extracts. Only functional active extracts were processed in the more time-consuming HRS mode, which was operated in combination with MS. Information on the number of active compounds, their retention times, the molecular masses, and the MS/MS-fingerprints as a function of their biological activity was obtained from 50% of the functional active extracts in real time. This dramatically enhances the speed of biologically active compound characterization in natural product extracts compared to traditional fractionation approaches.
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Akter, Shamoli, Md Abu Zubair, Md Shahinul Haque Khan, Luthfunnesa Bari, Md Azizul Huq, and Mohammad A. Rashid. "Identification and Quantification of Sodium Benzoate in Different Brands of Mango Juices Available in Tangail Region, Bangladesh." Bangladesh Pharmaceutical Journal 20, no. 1 (April 5, 2017): 20–26. http://dx.doi.org/10.3329/bpj.v20i1.32089.
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Chemical preservation has become an increasingly important practice in modern food technology. Sodium benzoate is a permitted food additive in restrictive amounts by international laws, but their content must be declared and must not exceed the established limits by legislation. An experimental study for the level of sodium benzoate in different brands of mango juices available in the markets, stores and shops in Tangail region of Bangladesh was determined by high performance liquid chromatography. A Luna 5 ? C18 (2) 100A column (250 × 4.6 mm) was used for the chromatographic analysis. Chromatographic separation was achieved with isocratic solvent system comprising of sodium acetate and acetic acid buffer (pH =4.0)/acetonitrile in the ratio of 80:20 (1 ml/min) at 37oC and the chromatograms were recorded at 254 nm. The limit of detection and quantification for sodium benzoate was 0.00076 mg/100 ml and 0.00231 mg/100 ml, respectively. Quantification of the selected brand juices revealed that the level of the used sodium benzoate was within the FDA standard range. But by comparing with the Bangladesh Standard and Testing Institute (BSTI), brand-1 and brand-3 of the analyzed juice samples was found to deviate the current legal limits. The percentage recovery was found to be 92.04 ± 1.98 to 98.01 ± 1.91. It was found that some of the brands used excess amount of sodium benzoate which may be harmful for our health.Bangladesh Pharmaceutical Journal 20(1): 20-26, 2017
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Vaingankar, Pradnya N., and Purnima D. Amin. "Development and Validation of Stability-Indicating RP-HPLC Method for Simultaneous Determination of Metformin HCI and Glimepiride in Fixed-Dose Combination." Analytical Chemistry Insights 11 (January 2016): ACI.S38137. http://dx.doi.org/10.4137/aci.s38137.
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A simple reversed-phase high-performance liquid chromatography method was developed and validated for simultaneous determination of Metformin hydrochloride (MET) and Glimepiride (GLM) in combination and estimation of their principal degradation products. The separation was achieved using JASCO Finepak SIL (250 mm × 4.6 mm i.d. 5 μm) at ambient temperature. The optimized mobile phase composed of an aqueous phase (20 mM phosphate buffer, adjusted to pH 3.0) and an organic phase (methanoliacetonitrile; 62.5:37.5) in the ratio of 80:20. The flow rate was 1 mL/minute, and the analytes were detected at 230 nm. The developed method was validated for accuracy, precision, specificity, linearity, and sensitivity. The chromatographic analysis time was approximately six minutes with the complete resolution of MET (Rt = 2.75 minutes) and GLM (Rt = 5.87 minutes). The method exhibited good linearity over the range of 5-30 μg/mL for MET and 1-10 μg/mL for GLM. The drugs in combination were subjected to various stress degradation studies as per the International Conference Harmonization (ICH) guidelines. Results obtained from the stress degradation studies revealed that the developed method is applicable for stability studies.
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Logoyda, Liliya, Yuliya Kondratova, Dmytro Korobko, and Yuriy Soroka. "DEVELOPMENT OF ULTRA-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF CAPTOPRIL IN PHARMACEUTICAL DOSAGE FORMS." Asian Journal of Pharmaceutical and Clinical Research 10, no. 11 (November 1, 2017): 308. http://dx.doi.org/10.22159/ajpcr.2017.v10i11.20462.
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Objective: The objective of this research was to develop more simple, sensitive, accurate, and less expensive analytical methods for the determination of captopril in medicines by Ultra-high-performance liquid chromatography.Materials and Methods: The chromatographic analysis of captopril performed on liquid chromatography Agilent 1290 Infinity II LC System.Results: A simple, rapid, sensitive, and specific method was developed for the determination of captopril by ultra-high-performance liquid chromatography in mono-medicines and pharmaceutical dosage forms in combination with hydrochlorothiazide without previous separation. Satisfactory resolution was achieved using Fused-Core® technology Ascentis Express C18 column (4.6×150 mm) and a mobile phase consisting of methanol and 0.1% solution of trifluoroacetic acid (40/60, v/v) at a flow rate 1.2 mL/minute and the wavelength detection was 220 nm. Ascentis Express columns, based on Fusеd-core pаrticle technоlogy, prоvide more than twice the speed and efficiency of traditiоnal cоlumns at half the backpressure of sub-2-μm columns. The retention time for captopril was 1.345 minute. The validation of this method was based on the ICH and USP guidelines.Conclusion: The results obtained in this research work clearly indicated that the assay was rapid, sensitive and successfully applied to the determination of both drugs in pharmaceutical dosage forms without interference from tablet excipients.
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Strube, A., A. Buettner, and Carola Groetzinger. "Characterization and identification of a plastic-like off-odor in mineral water." Water Supply 9, no. 3 (August 1, 2009): 299–309. http://dx.doi.org/10.2166/ws.2009.382.
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A specific mineral water off-odor, the so-called “sunlight” flavor produced after UV light exposure, was characterized by sensory analysis in different mineral water samples and ranked according to overall odor intensity. The odorants were isolated by means of solvent extraction and stir bar sorptive extraction (SBSE) techniques, respectively. Analyses were performed with two-dimensional (2D) high resolution gas chromatographic (HRGC) separation and parallel mass spectrometric (MS) and olfactometric (O) detection. Additionally, analyses of off-odor-free samples exposed to natural sunlight or to “artificial” UV radiation (replicating natural sunlight) were analyzed to assess off-odor compound formation. 14 common characteristic odorants in commercial off-odor and irradiated samples were identified. These were predominantly saturated and mono or di-unsaturated carbonyl compounds, with several substances exhibiting the characteristic fatty and plastic-like odor impressions. Eight of the compounds identified were detected for the first time as off-odor “sunlight” flavor contributors to mineral water and had amongst the highest flavor dilution (FD) factors in the extracted samples.
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Schröder, H. Fr. "Identification of Non-Biodegradable, Hydrophilic, Organic Substances in Industrial and Municipal Waste Water Treatment Plant-Effluents by Liquid Chromatography-Tandem Mass Spectrometry (LC/MS/MS)." Water Science and Technology 23, no. 1-3 (January 1, 1991): 339–47. http://dx.doi.org/10.2166/wst.1991.0432.
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Effluents of biological waste water treatment plants containing high concentrations of non-biodegradable substances measured as COD (chemical oxygen demand) were analyzed by gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS). GC/MS could detect any relevant compound because of involatility of these substances. LC/MS/MS was able to give molecular weight information without any separation bypassing analytical column. Daughter- and parent-ions formed by MS/MS gave structural information by fragmentation under CID-conditions (collisionally induced dissociation) even for UV-non-detectable chromophor missing substances. Metabolites and anthropogenic, non-biodegradable substances such as polyether, nonionic alkyl-and arylsurfactants and benzene-sulfonic acid could be detected and identified after C 18 column separation and without any prior separation, bypassing column. Analysis without any separation could be done within a few minutes up to an hour, column separation lasted 10 to 100 fold longer.
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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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Schwedhelm, Edzard. "Quantification of ADMA: analytical approaches." Vascular Medicine 10, no. 2_suppl (May 2005): S89—S95. http://dx.doi.org/10.1191/1358863x05vm596oa.
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Methylated L-arginine analogs are involved in nitric oxide synthase activity regulation. Methods based on high-performance liquid chromatography with fluorescence, capillary electrophoresis, or ion exchange chromatography with absorbance detection were first applied for the quantitative determination of N-monomethyl-L-arginine (NMMA), asymmetric dimethylarginine (ADMA) and symmetric dimethylarginine (SDMA) in human blood and urine. These assays revealed elevated circulating levels of ADMA in various diseases and gave accumulating evidence of the usefulness of ADMA as a cardiovascular risk factor. However, the methods used are hampered by the fact that NMMA, ADMA and SDMA can be distinguished from L-arginine only by means of chromatographic separation. This has promoted the development of alternatives that involve mass spectrometry (MS) technology. Today, various MS-based approaches such as liquid chromatography (LC)-MS, LC-MS/MS, gas chromatography (GC)-MS, and GC-MS/MS are available. L-arginine and its analogs have been subjected to LC-MS analysis with and without further derivatization to their o-phthaldialdehyde derivatives. For these methods, labelled L-arginine was used as the internal standard. The first MS-based method that distinguishes NMMA, ADMA, SDMA and L-arginine by mass-to-charge (m/z)- ratio has been reported by Tsikas et al. This GC-MS approach has been further improved by Albsmeier et al by introducing labelled ADMA as an internal standard. As an alternative to existing methods, a commercially available ELISA kit has recently been developed and validated.
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Schwedhelm, Edzard. "Quantification of ADMA: analytical approaches." Vascular Medicine 10, no. 1_suppl (July 2005): S89—S95. http://dx.doi.org/10.1177/1358836x0501000113.
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Methylated L-arginine analogs are involved in nitric oxide synthase activity regulation. Methods based on high-performance liquid chromatography with fluorescence, capillary electrophoresis, or ion exchange chromatography with absorbance detection were first applied for the quantitative determination of N-monomethyl-L-arginine (NMMA), asymmetric dimethylarginine (ADMA) and sym metric dimethylarginine (SDMA) in human blood and urine. These assays revealed elevated circulating levels of ADMA in various diseases and gave accumulating evidence of the usefulness of ADMA as a cardiovascular risk factor. However, the methods used are hampered by the fact that NMMA, ADMA and SDMA can be dis tinguished from L-arginine only by means of chromatographic separation. This has promoted the development of alternatives that involve mass spectrometry (MS) technology. Today, various MS-based approaches such as liquid chromatography (LC)-MS, LC-MS/MS, gas chromatography (GC)-MS, and GC-MS/MS are available. L-arginine and its analogs have been subjected to LC-MS analysis with and without further derivatization to their o-phthaldialdehyde derivatives. For these methods, labelled L-arginine was used as the internal standard. The first MS-based method that distinguishes NMMA, ADMA, SDMA and L-arginine by mass-to-charge (m/z)- ratio has been reported by Tsikas et al. This GC-MS approach has been further improved by Albsmeier et al by introducing labelled ADMA as an internal standard. As an alternative to existing methods, a commercially available ELISA kit has recently been developed and validated.
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Yanamandra, Ramesh, Avinash Chaudhary, Srinivasa Rao Bandaru, Balaram Patro, Y. L. N. Murthy, Parimi Atchuta Ramaiah, and C. S. P. Sastry. "UPLC Method for Simultaneous Separation and Estimation of Secnidazole, Fluconazole and Azithromycin in Pharmaceutical Dosage Forms." E-Journal of Chemistry 7, s1 (2010): S363—S371. http://dx.doi.org/10.1155/2010/235186.
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A novel approach was carried out to develop and validate a rapid, specific, accurate and precise reverse phase ultra performance liquid chromatographic (UPLC) method for the simultaneous separation and quantification of secnidazole, fluconazole and azithromycin in pharmaceutical dosage forms. The developed analytical method is superior in technology to conventional HPLC with respect to time, resolution, solvent consumption and cost of analysis. Elution time for the separation was 10 min and ultra violet detection was carried out at 210 nm. Efficient separation was achieved on BEH C18 sub-2-μm UPLC column using 0.002 M Na2HPO4and acetonitrile as organic solvent in a gradient program. Benzophenone was used as internal standard. Resolutions between secnidazole, fluconazole and azithromycin were found to be more than 4.8. The calibration graphs were linear for secnidazole, fluconazole, benzophenone and azithromycin. The method showed excellent recoveries for all dosage forms. The test solution was found to be stable in diluent for 72 h when stored in the refrigerator between 2 to 8°C. The proposed UPLC method was validated with respect to linearity, accuracy, precision, specificity and robustness and can be used for the simultaneous estimation of secnidazole, fluconazole and azithromycin in tablet dosage forms available as a combi kit.
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Hernández-Mesa, Maykel, David Ropartz, Ana M. García-Campaña, Hélène Rogniaux, Gaud Dervilly-Pinel, and Bruno Le Bizec. "Ion Mobility Spectrometry in Food Analysis: Principles, Current Applications and Future Trends." Molecules 24, no. 15 (July 25, 2019): 2706. http://dx.doi.org/10.3390/molecules24152706.
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In the last decade, ion mobility spectrometry (IMS) has reemerged as an analytical separation technique, especially due to the commercialization of ion mobility mass spectrometers. Its applicability has been extended beyond classical applications such as the determination of chemical warfare agents and nowadays it is widely used for the characterization of biomolecules (e.g., proteins, glycans, lipids, etc.) and, more recently, of small molecules (e.g., metabolites, xenobiotics, etc.). Following this trend, the interest in this technique is growing among researchers from different fields including food science. Several advantages are attributed to IMS when integrated in traditional liquid chromatography (LC) and gas chromatography (GC) mass spectrometry (MS) workflows: (1) it improves method selectivity by providing an additional separation dimension that allows the separation of isobaric and isomeric compounds; (2) it increases method sensitivity by isolating the compounds of interest from background noise; (3) and it provides complementary information to mass spectra and retention time, the so-called collision cross section (CCS), so compounds can be identified with more confidence, either in targeted or non-targeted approaches. In this context, the number of applications focused on food analysis has increased exponentially in the last few years. This review provides an overview of the current status of IMS technology and its applicability in different areas of food analysis (i.e., food composition, process control, authentication, adulteration and safety).
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Ahmad, Jameel. "The Use of Impregnated Silica Gel Layers and Modified Celluloses in Thin-Layer Chromatographic Analysis of Inorganic Mixtures." Separation Science and Technology 30, no. 12 (July 1995): 2429–54. http://dx.doi.org/10.1080/01496399508021394.
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Hansa, A., V. L. Pillay, and C. A. Buckley. "Analysis of reactive dyes using high performance capillary electrophoresis." Water Science and Technology 39, no. 10-11 (May 1, 1999): 169–72. http://dx.doi.org/10.2166/wst.1999.0649.
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Increasing reports of coloured effluent from waste water treatment plants receiving reactive dye waste from textile mills indicate the need to learn more about the fate of these dyes. The project concerns the development of analytical techniques for the analysis of reactive dyes in textile waste. An analytical procedure using High Performance Capillary Electrophoresis (HPCE) and High Performance Liquid Chromatography (HPLC) for the separation of a range of reactive dyes in textile waste water is described. The dyes belong to a range of bis-monochlorotriazinyl dyes used widely in the dyeing of cotton textiles.
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Amaral, Michelle S. S., and Philip J. Marriott. "The Blossoming of Technology for the Analysis of Complex Aroma Bouquets—A Review on Flavour and Odorant Multidimensional and Comprehensive Gas Chromatography Applications." Molecules 24, no. 11 (May 31, 2019): 2080. http://dx.doi.org/10.3390/molecules24112080.
Full textAbstract:
Multidimensional approaches in gas chromatography have been established as potent tools to (almost) attain fully resolved analyses. Flavours and odours are important application fields for these techniques since they include complex matrices, and are of interest for both scientific study and to consumers. This article is a review of the main research studies in the above theme, discussing the achievements and challenges that demonstrate a maturing of analytical separation technology.
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Li, H. Q., and H. F. Schröder. "Surfactants – standard determination methods in comparison with substance specific mass spectrometric methods and toxicity testing by Daphnia magna and Vibrio fischeri." Water Science and Technology 42, no. 7-8 (October 1, 2000): 391–98. http://dx.doi.org/10.2166/wst.2000.0593.
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The recovery of different types of surfactants formerly applied and up-coming new ones from spiked wastewater and ultra-pure water was examined by sum parameter determinations (substance-group-specific Methylene Blue (MBAS), Bismuth Active (BiAS) and Disulfine Blue Active Substances (DSBAS)) and by substance-specific mass spectrometric detection (MS). For MS determination atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) was applied in the flow injection (FIA) and liquid chromatographic separation (LC) mode. Quantitation was performed in the multiple ion detection mode using mass and tandem (MS/MS) mass spectrometric detection. In parallel the ecotoxicological potential of these surfactants was determined by Daphnia magna and Vibrio fischeri toxicity testing. MS was found to provide more reliable data in surfactant analysis than the substance-group-specific methods. The toxicity of the up-coming new surfactants against water organisms should not be neglected.