Journal articles: 'Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry (UHPLC-MS/MS)'

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Chen, Wen-Ling, Tzu-Fang Hsu, and Chia-Yang Chen. "Performance Liquid Chromatography/Tandem Mass Spectrometry." Journal of AOAC INTERNATIONAL 94, no. 3 (May 1, 2011): 872–77. http://dx.doi.org/10.1093/jaoac/94.3.872.

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Abstract A sensitive method was developed using ultra-high-performance liquid chromatography (UHPLC)/MS/MS with positive electrospray ionization for determining aflatoxin M1 (AFM1) in milk and milk powder. A 50 mL quantity of low-fat liquid milk containing 100 ng/L AFM1 was prepared using immunoaffinity columns with a mean recovery rate of 79% (n = 3). UHPLC columns (BEH C18, BEH HILIC, and HSS T3) greatly reduced the chromatographic time and lowered the instrumental detection limits (IDLs) 16 to 58 times compared to an HPLC column (Betabasic C18). The HSS T3 column was chosen because it provided a low IDL (0.11 pg) and the lowest ion suppression of signal intensity (63.4%) among the tested columns. Matrix-fortified calibration curves were used for quantification and showed good linearity (r > 0.997) at 0.05–500 ng/mL. The LOD was 0.18 ng/kg for milk and 2.08 ng/kg for milk powder, based on the signal intensity of the confirmatory product ion (m/z 259.1), which was less abundant than the quantitative product ion (m/z 273.1). Certified reference materials of milk powder

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Bayer, O. V., O. V. Kaminska, O. V. Bondarets, O. S. Yaremchuk, O. I. Skoromna, S. V. Midyk, L. V. Shevchenko, V. M. Mykhalska, O. M. Stupak, and N. V. Liniichuk. "Evaluation of Ultra-High-Performance Liquid Chromatography (HPLC) Tandem Mass Spectrometry for Determination of Avermectin Residues in Milk." Ukrainian Journal of Ecology 9, no. 4 (December 7, 2019): 521–26. http://dx.doi.org/10.15421/2019_784.

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The study was conducted to evaluate the applicability of ultra high-performance liquid chromatography - tandem mass spectrometry method (UHPLC-MS/MS), establish the MS/MS detection parameters and determine the validation characteristics for the analysis of residual content of avermectins in milk. The UHPLC-MS/MS method has proved to be accurate, practical and universal. This was confirmed by Decision limit (CCα) data: abamectin - 12.56 μg/kg, doramectin - 17.74 μg/kg, eprinomectin - 24.02 μg/kg, ivermectin - 12.53 μg/kg, moxidectin - 44.69 μg/kg, recovery is 88.7-110%. The data obtained for assessing the suitability, accuracy and reproducibility of the results meet the requirements of the European Directive (2002/657/EC). The efficient ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method that was developed and adopted for routine use by the laboratories of veterinary medicine, allows to detect residual quantities of 5 avermectins used in animal breeding for the prevention of helminthiases in food products including milk.

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Faccin, Henrique, Roberta Fabricio Loose, Carine Viana, Osmar A. Lameira, and Leandro Machado de Carvalho. "Determination of phenolic compounds in extracts of Amazonian medicinal plants by liquid chromatography-electrospray tandem mass spectrometry." Analytical Methods 9, no. 7 (2017): 1141–51. http://dx.doi.org/10.1039/c6ay02937j.

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A method for the separation, identification and quantification of 24 phenolic compounds using ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed and validated.

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Nie, Xu-Heng, and Hua-Chun Guo. "An ultra-high-performance liquid chromatography-triple quadrupole mass spectrometry method for the detection of steroidal glycoalkaloids in potato samples." Analytical Methods 9, no. 47 (2017): 6613–21. http://dx.doi.org/10.1039/c7ay02244a.

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An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method has been optimized and validated to simultaneously monitor steroidal glycoalkaloids (SGAs), α-chaconine and α-solanine, in potato samples stored under natural indoor conditions in Kunming.

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Wang, Jian, Wendy Cheung, and Willis Chow. "Ultra-High Performance Liquid Chromatography/Electrospray Ionization-Tandem Mass Spectrometry Determination of 151 Pesticides in Soybeans and Pulses." Journal of AOAC INTERNATIONAL 96, no. 5 (September 1, 2013): 1114–33. http://dx.doi.org/10.5740/jaoacint.12-465.

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Abstract This paper presents the application of ultra-high performance LC (UHPLC) and MS for the determination of 151 pesticides in soybeans and pulses. A core-shell particle (2.6 μm particle size) column and a fully porous sub-2 μm (1.7 μm particle size) column showed comparable performance in chromatographic resolution and separation, increasing selectivity, and reducing analysis time. UHPLC was coupled with either a triple quadrupole mass analyzer (MS/MS) or a quadrupole Orbitrap (namely Orbital trap) mass spectrometer (Q-Orbitrap MS), which possesses fast data acquisition capability. Both configurations yielded analytical run times of ≤14 min. Soybean and pulse samples were analyzed and quantitated for pesticide residues using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure, UHPLC/electrospray ionization (ESI)-MS/MS, and matrix-matched standard calibration curves (in an analytical range of 5–500 μg/kg) with isotopically-labeled standards or a chemical analog as internal standards. The method performance parameters that included overall recovery, intermediate precision, and measurement uncertainty were evaluated according to a nested design experiment. Approximately 89% of the pesticides studied had recoveries between 81 and 110%; 95%, had intermediate precision ≤20%; and 93% showed measurement uncertainty ≤40%. From a pilot study of 100 samples, eight tested positive by UHPLC/ESI-MS/MS for carbendazim, methomyl, or imidacloprid. These pesticides were further confirmed using UHPLC/ESI-Q-Orbitrap MS based on accurate mass measurement with mass error ≤5 ppm.

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Nannapaneni, Nagaraj Kumar, Sunil S. Jalalpure, Rajendraprasad Muppavarapu, and Sunil Kumar Sirigiri. "An ultra high performance liquid chromatography-tandem mass spectrometry method for the quantification of linagliptin in human plasma." RSC Advances 6, no. 71 (2016): 66756–66. http://dx.doi.org/10.1039/c6ra10450a.

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Wang, Xiao Fang, Chun Liang Yang, Mao Fang Huang, Ming Yue Wang, Yu Bing Zha, Ling Lin, and Shao Dong Zeng. "Determination of Diflubenzuron Residues in Vegetables by UPLC-MS/MS." Advanced Materials Research 852 (January 2014): 266–69. http://dx.doi.org/10.4028/www.scientific.net/amr.852.266.

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The conditions for detecting residues of diflubenzuron in vegetables by ultra high performance liquid chromatography tandem mass spectrometry were studied. The target was extracted with acetonitrile for 2 min with a homogenizer. The extaction was purifide by a conditioned Florisil SPE cartridge, and then was detected by ultra high-performance liquid chromatography with tandem mass spectrometry. The average recovery was in the range from 87.8 %- 99.2 % at spike levels of 0.1, 1.0 and 10 mg/kg in vegetables, and relative standard deviations was in the range of 4.2 %-8.9 %. The proposed method is fast, simple, sensitive and accurate.

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Pezzatti, Julian, Víctor González-Ruiz, Julien Boccard, Davy Guillarme, and Serge Rudaz. "Evaluation of Different Tandem MS Acquisition Modes to Support Metabolite Annotation in Human Plasma Using Ultra High-Performance Liquid Chromatography High-Resolution Mass Spectrometry for Untargeted Metabolomics." Metabolites 10, no. 11 (November 15, 2020): 464. http://dx.doi.org/10.3390/metabo10110464.

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Ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS) is a powerful and essential technique for metabolite annotation in untargeted metabolomic applications. The aim of this study was to evaluate the performance of diverse tandem MS (MS/MS) acquisition modes, i.e., all ion fragmentation (AIF) and data-dependent analysis (DDA), with and without ion mobility spectrometry (IM), to annotate metabolites in human plasma. The influence of the LC separation was also evaluated by comparing the performance of MS/MS acquisition in combination with three complementary chromatographic separation modes: reversed-phase chromatography (RPLC) and hydrophilic interaction chromatography (HILIC) with either an amide (aHILIC) or a zwitterionic (zHILIC) stationary phase. RPLC conditions were first chosen to investigate all the tandem MS modes, and we found out that DDA did not provide a significant additional amount of chemical coverage and that cleaner MS/MS spectra can be obtained by performing AIF acquisitions in combination with IM. Finally, we were able to annotate 338 unique metabolites and demonstrated that zHILIC was a powerful complementary approach to both the RPLC and aHILIC chromatographic modes. Moreover, a better analytical throughput was reached for an almost negligible loss of metabolite coverage when IM-AIF and AIF using ramped instead of fixed collision energies were used.

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Fical, Luboš, Maria Khalikova, Hana Kočová Vlčková, Ivona Lhotská, Zuzana Hadysová, Ivan Vokřál, Lukáš Červený, František Švec, and Lucie Nováková. "Determination of Antiviral Drugs and Their Metabolites Using Micro-Solid Phase Extraction and UHPLC-MS/MS in Reversed-Phase and Hydrophilic Interaction Chromatography Modes." Molecules 26, no. 8 (April 7, 2021): 2123. http://dx.doi.org/10.3390/molecules26082123.

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Two new ultra-high performance liquid chromatography (UHPLC) methods for analyzing 21 selected antivirals and their metabolites were optimized, including sample preparation step, LC separation conditions, and tandem mass spectrometry detection. Micro-solid phase extraction in pipette tips was used to extract antivirals from the biological material of Hanks balanced salt medium of pH 7.4 and 6.5. These media were used in experiments to evaluate the membrane transport of antiviral drugs. Challenging diversity of physicochemical properties was overcome using combined sorbent composed of C18 and ion exchange moiety, which finally allowed to cover the whole range of tested antivirals. For separation, reversed-phase (RP) chromatography and hydrophilic interaction liquid chromatography (HILIC), were optimized using extensive screening of stationary and mobile phase combinations. Optimized RP-UHPLC separation was carried out using BEH Shield RP18 stationary phase and gradient elution with 25 mmol/L formic acid in acetonitrile and in water. HILIC separation was accomplished with a Cortecs HILIC column and gradient elution with 25 mmol/L ammonium formate pH 3 and acetonitrile. Tandem mass spectrometry (MS/MS) conditions were optimized in both chromatographic modes, but obtained results revealed only a little difference in parameters of capillary voltage and cone voltage. While RP-UHPLC-MS/MS exhibited superior separation selectivity, HILIC-UHPLC-MS/MS has shown substantially higher sensitivity of two orders of magnitude for many compounds. Method validation results indicated that HILIC mode was more suitable for multianalyte methods. Despite better separation selectivity achieved in RP-UHPLC-MS/MS, the matrix effects were noticed while using both chromatographic modes leading to signal enhancement in RP and signal suppression in HILIC.

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Cabañas-García, Emmanuel, Carlos Areche, Juan Jáuregui-Rincón, Francisco Cruz-Sosa, and Eugenio Pérez-Molphe Balch. "Phytochemical Profiling of Coryphantha macromeris (Cactaceae) Growing in Greenhouse Conditions Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry." Molecules 24, no. 4 (February 15, 2019): 705. http://dx.doi.org/10.3390/molecules24040705.

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Chromatographic separation combined with mass spectrometry is a powerful tool for the characterization of plant metabolites because of its high sensitivity and selectivity. In this work, the phytochemical profile of aerial and radicular parts of Coryphantha macromeris (Engelm.) Britton & Rose growing under greenhouse conditions was qualitatively investigated for the first time by means of modern ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-PDA-HESI-Orbitrap-MS/MS). The UHPLC-PDA-HESI-Orbitrap-MS/MS analysis indicated a high complexity in phenolic metabolites. In our investigation, 69 compounds were detected and 60 of them were identified. Among detected compounds, several phenolic acids, phenolic glycosides, and organic acids were found. Within this diversity, 26 metabolites were exclusively detected in the aerial part, and 19 in the roots. Twenty-four metabolites occurred in both plant parts. According to the relative abundance of peaks in the chromatogram, ferulic and piscidic acids and their derivatives may correspond to one of the main phenolic compounds of C. macromeris. Our results contribute to the phytochemical knowledge regarding C. macromeris and its potential applications in the pharmaceutical and cosmetic industries. Besides, some metabolites and their fragmentation patterns are reported here for the first time for cacti species.

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Zhu, Difeng, Li Ping, Yawen Hong, Jiale Shen, Qinjie Weng, and Qiaojun He. "Simultaneous Quantification and Pharmacokinetic Study of Five Homologs of Dalbavancin in Rat Plasma Using UHPLC-MS/MS." Molecules 25, no. 18 (September 8, 2020): 4100. http://dx.doi.org/10.3390/molecules25184100.

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Dalbavancin is a novel semisynthetic glycopeptide antibiotic that comprises multiple homologs and isomers of similar polarities. However, pharmacokinetic studies have only analyzed the primary components of dalbavancin, namely B0 and B1. In this study, an ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed to simultaneously determinate and investigate the five homologous components of dalbavancin, namely, A0, A1, B0, B1, and B2, in rat plasma. In this method, methanol was used to precipitate plasma, and a triple-bonded alkyl chromatographic column was used for molecule separation, using 0.1% formic acid-acetonitrile as the mobile phase for gradient elution. Targeted homologs were analyzed by a triple quadrupole mass spectrometer using positive electrospray ionization in multiple reaction monitoring mode. The linearity range was 50–2500 ng/mL with a high correlation coefficient (r2 > 0.998). This method was successfully applied in the pharmacokinetic analysis of dalbavancin hydrochloride to investigate dalbavancin components in rats.

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Huang, Yu-Fang, Yi-Min Huang, and Hsin-Jui Lee. "Simultaneous Analysis of Seven Neonicotinoids in Commercial Milk Samples Using an UHPLC-MS/MS Method." Applied Sciences 10, no. 19 (September 27, 2020): 6775. http://dx.doi.org/10.3390/app10196775.

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A liquid–liquid extraction and ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS) method was developed for simultaneous analysis of the residues of seven neonicotinoid insecticides (NEOs), namely acetamiprid, clothianidin, dinotefuran, imidacloprid, thiacloprid, thiamethoxam, and nitenpyram, in commercial milk samples. The method had a good linearity (R2 > 0.992) and a limit of detection range of 0.004–0.15 μg/kg. The average recovery range was 89–119% with an intraday precision of 1.4–10.3% at spiking levels of 8, 12, and 16 μg/kg. The validated method was employed for routine analysis of the aforementioned seven NEOs in commercial milk samples obtained randomly from a supermarket in Miaoli (Taiwan). The detected thiamethoxam and clothianidin levels were 3.4 and 80 μg/kg, respectively.

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Shi, Zhihong, Xinye Li, Hongyu Ma, Weiyue Pang, Yamei Sun, Yifan He, Meiting Li, and Hongyi Zhang. "Determination of seven phenolic acids in honey by counter flow salting-out homogeneous liquid–liquid extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry." Analytical Methods 11, no. 31 (2019): 4044–51. http://dx.doi.org/10.1039/c9ay01492f.

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Mas-Capdevila, Anna, Lisard Iglesias-Carres, Anna Arola-Arnal, Gerard Aragonès, Begoña Muguerza, and Francisca Isabel Bravo. "Implication of Opioid Receptors in the Antihypertensive Effect of a Novel Chicken Foot-Derived Peptide." Biomolecules 10, no. 7 (July 2, 2020): 992. http://dx.doi.org/10.3390/biom10070992.

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The peptide AVFQHNCQE demonstrated to produce nitric oxide-mediated antihypertensive effect. This study investigates the bioavailability and the opioid-like activity of this peptide after its oral administration. For this purpose, in silico and in vitro approaches were used to study the peptide susceptibility to GI digestion. In addition, AVFQHNCQE absorption was studied both in vitro by using Caco-2 cell monolayers and in vivo evaluating peptide presence in plasma from Wistar rats by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and by ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS). Both in vivo and in vitro experiments demonstrated that peptide AVFQHNCQE was not absorbed. Thus, the potential involvement of opioid receptors in the BP-lowering effect of AVFQHNCQE was studied in the presence of opioid receptors-antagonist Naloxone. No changes in blood pressure were recorded in rats administered Naloxone, demonstrating that AVFQHNCQE antihypertensive effect is mediated through its interaction with opioid receptors. AVFQHNCQE opioid-like activity would clarify the antihypertensive properties of AVFQHNCQE despite its lack of absorption.

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Gervasoni, Jacopo, Aniello Primiano, Cristina Graziani, Franco Scaldaferri, Antonio Gasbarrini, Andrea Urbani, and Silvia Persichilli. "Validation of UPLC-MS/MS Method for Determination of Urinary Lactulose/Mannitol." Molecules 23, no. 10 (October 20, 2018): 2705. http://dx.doi.org/10.3390/molecules23102705.

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Determination of urinary lactulose/mannitol is one of the most used tests to evaluate intestinal barrier function. High-performance liquid chromatography (HPLC) separation with electrospray ionization tandem mass spectrometry guarantees high levels of selectivity and reproducibility. In this paper we report an upgrade of the previous published liquid chromatography tandem mass spectrometry method, introducing more reliable internal standards and ultra-performance liquid chromatography with ethylene bridged hybrid amide columns. The ultra-performance liquid chromatography provided an efficient chromatographic separation of the two sugars in 5 min, compared to 15 min using the previous method. The limit of quantification was 10 µg/mL for mannitol and 2.5 µg/mL for lactulose, and the assay was linear up to 1000 µg/mL for mannitol and 1000 µg/mL for lactulose. The within-run precision and accuracy ranged from 0.7 to 2.9% and 97.2 to 101.2%, respectively. The between-run precision and accuracy ranged from 1.9 to 4.7% and 94.8 to 97.5%, respectively. Recovery was higher than 90.2% for both lactulose and mannitol, and the matrix effect for both lactulose and mannitol was lower than 15%. With this new method we have a real improvement in terms of accuracy and reproducibility, ensuring results in shorter time. The changes to the previous protocol make this method excellent for routine purposes.

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Kataev, S. S., O. N. Dvorskaya, M. A. Gofenberg, A. V. Labutin, and A. B. Melentyev. "ANALYTICAL FEATURES OF SYNTHETIC MDMB(N)-073F CANNABIMIMETICS AND ITS MARKERS IN BIOLOGICAL MATERIAL." Pharmacy & Pharmacology 7, no. 4 (September 10, 2019): 184–97. http://dx.doi.org/10.19163/2307-9266-2019-7-4-184-197.

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The aim of the research is to study both analytical features of synthetic MDMB(N)-073F cannabimimetics of indazole carboxamides group by gas chromatography methods combined with tandem mass spectrometry (GC-MS) and high performance liquid chromatography with high-resolution mass spectrometry (HPLC-HRMS) as well as characteristics of the major MDMB(N)-073F metabolite, its glucuronide and derivatives, using gas chromatography with mass-spectrometric (GC-MS) detection and high-performance liquid chromatography (HPLC) with MS/MS mass spectrometry (HPLC-MS/MS) in urine samples to be applied in expert practice, chemical-toxicological and forensic and chemical analyses.Materials and methods. To carry out the study, the following materials were used: plant-based objects with narcotic drugs withdrawn from illegal trafficking and applied to them;. urine samples to be studied under chemical-toxicological and forensic and chemical analyses. For solid-phase epitaxy, SampliQ EVIDEX TFE cartridges – 200 mg – 3 ml (Agilent, USA) were used for sample preparation; β-glucuronidase, Type HP-2, From Helix Pomatia, 100000 UA/ml (Sigma-ALDRICH CHEMI, Germany) was used for enzymatic hydrolysis. GC-MS/MS analysis was made using Agilent 7890 gas chromatograph with a tandem quadrupolar mass-spectrometer Agilent 7000 (Agilent, США); GC-MS analysis was carrid out using gas chromatograph Agilent 7820 with mass-selective detector Agilent 5975 (Agilent, USA); HPLC-HRMS research was made on liquid chromatograph Agilent 1260 with tandem hybrid high-resolution quadrupole-time-of-flight detector Agilent 6540 (Agilent, США); liquid chromatograph Agilent 1260 with Agilent 6460 (Agilent, USA) with tandem mass-spectrometer were used for making HPLC-MS/MS research.Results. The structure of MDMB(N)-073F compound has been confirmed and an exact mass of the protonated molecule corresponding to the chemical formula C19H27FN3O3 fixed by GC-MS/MS and HPLC-HRMS methods. Spectral characteristics of MDMB(N)-073F have been given. One of the branches in MDMB(N)-073F biotransformation in the human body found out by GC-MS and HPLC-MS/MS methods, is the ester decomposition with further conjugation of the resulting acid. The product interacting with glucuronic acid, is found to be the conjugate of major MDMB(N)-073F metabolite of the Ist phase in biotransformation. Metabolites appearing due to the ester decomposition and its conjugate with glucuronic acid, are recommended to be used as markers for synthetic MDMB(N)-073F cannabimimetics in the analysis by chromatographic methods; they can be used for regular screening of biological samples.Conclusion. The research results presented here, are the following: the analytical features characteristic for synthetic MDMB(N)-073F cannabimimetics found out by gas chromatography methods combined with tandem mass spectrometry (GC-MS/ MS) and liquid chromatography of hybrid high-resolution quadrupole-time-of-flight mass spectrometry (HPLC-HRMS), as well as characteristics of major MDMB(N)-073F metabolite, its glucuronide and derivatives with the use of gas chromatography with mass-spectrometric detection (GC-MS) and liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS) in urine samples to be applied in expert practice, chemical-toxicological, forensic and chemical analyses.

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Huang, Min, Doug Winters, Darryl Sullivan, and Dawn Dowell. "Application of Ultra-High-Performance Liquid Chromatography/ Tandem Mass Spectrometry for the Measurement of Vitamin D in Infant Formula and Adult/Pediatric Nutritional Formula: First Action 2011.11." Journal of AOAC INTERNATIONAL 95, no. 2 (March 1, 2012): 319–21. http://dx.doi.org/10.5740/jaoacint.cs2011_11.

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Abstract In an effort to measure vitamin D, ultra-high- performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) was applied to samples. The use of UHPLC-MS/MS decreased the run time by 50%. The UHPLC-MS/MS achieved equal or better separation efficiency with complex food matrixes compared to HPLC-MS/MS. It was also observed that under the optimized conditions of UHPLC, all previtamins of vitamin D3, D2, and isotope-labeled vitamin D3 were baseline- separated from their corresponding vitamins. The sterol isomers found in complex food matrixes that interfere in the analysis were well separated from the analytes. The accuracy of the method was evaluated by analyzing National Institute of Standards and Technology Standard Reference Material 1849 infant reference material. The average vitamin D3 concentration was 0.251 ± 0.012 μg/g. This showed excellent agreement with the certified value of 0.251 ± 0.027 μg/g. The spike recovery study of a commercial infant formula matrix showed a range of recovery from 100 to 108%. The LOQ values determined were 0.0022 and 0.0028 μg/g for vitamins D3 and D2, respectively; LOD values were 0.00065 and 0.00083 μg/g for vitamins D3 and D2, respectively.

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Nualkaw, Kraiwut, Saranya Poapolathep, Zhaowei Zhang, Qi Zhang, Mario Giorgi, Peiwu Li, Antonio Francesco Logrieco, and Amnart Poapolathep. "Simultaneous Determination of Multiple Mycotoxins in Swine, Poultry and Dairy Feeds Using Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry." Toxins 12, no. 4 (April 13, 2020): 253. http://dx.doi.org/10.3390/toxins12040253.

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A reliable, sensitive and accurate multiple mycotoxin method was developed for the simultaneous determination of 17 mycotoxins in swine, poultry and dairy feeds using stable isotope dilution (13C-ISTD) and (ultra)-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A simple QuEChERS-based method (quick, easy, cheap, effective, rugged and safe) was developed consisting of soaking with a solution of 1% formic acid followed by extraction with acetonitrile, clean-up with C18 sorbent and finally adding 13C-ISTD before the UHPLC-MS/MS analysis. The chromatographic condition was optimized for separation and detection of the 17 mycotoxins using gradient elution. The method’s performance complied with the SANTE/11813/2017 standard and had mean recovery accuracies in the range 70%–120% and precision testing of % relative standard deviation (RSD) ≤ 20%. The limit of detection and limit of quantification values ranged from 0.25 to 40.0 ng/g and 0.5 to 100.0 ng/g, respectively. Finally, the method was applied to analyze feed samples, with the results showing that fumonisins, zearalenone, aflatoxin B1 and deoxynivalenol were the most prevalent mycotoxins contaminating the feed samples.

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Zhang, Liang, Yuhui Han, Jinjun Shan, Yuhong Liang, Liwei Xu, Shihua Zhang, Junsong Li, and Xiaochun Wan. "Simultaneous determination of seven catechins in rat plasma by ultra-high performance liquid chromatography tandem mass spectrometry and its application to a pharmacokinetics study." Analytical Methods 7, no. 22 (2015): 9415–20. http://dx.doi.org/10.1039/c5ay01766a.

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Pantano, Licia, Ladislao La Scala, Francesco Olibrio, Francesco Giuseppe Galluzzo, Carmelo Bongiorno, Maria Drussilla Buscemi, Andrea Macaluso, and Antonio Vella. "QuEChERS LC–MS/MS Screening Method for Mycotoxin Detection in Cereal Products and Spices." International Journal of Environmental Research and Public Health 18, no. 7 (April 4, 2021): 3774. http://dx.doi.org/10.3390/ijerph18073774.

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We developed and validated a screening method for mycotoxin analysis in cereal products and spices. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS) was used for the analysis. Dispersive solid-phase extractions (d-SPEs) were used for the extraction of samples. Ochratoxin A (OTA), zearalenone (ZEA), aflatoxins (AFLA; AFB1, AFB2, AFG1, AFG2), deoxynivalenol (DON), fumonisin (FUMO; FB1, FB2, FB3), T2, and HT2 were validated in maize. AFLA and DON were validated in black pepper. The method satisfies the requirements of Commission Regulation (EC) no. 401/2006 and (EC) no. 1881/2006. The screening target concentration (STC) was under maximum permitted levels (MLs) for all mycotoxins validated. The method’s performance was assessed by two different proficiencies and tested with 100 real samples.

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Ma, Shuping, Xiu Ye, Peiting Huang, Longshan Zhao, and Ning Liang. "Simultaneous determination of nitroimidazoles and amphenicol antibiotics in water samples using ultrasound-assisted dispersive liquid–liquid microextraction coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry." Analytical Methods 8, no. 46 (2016): 8219–26. http://dx.doi.org/10.1039/c6ay02465c.

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Ji, Huoyan, Lei Shen, Xiuying Shi, Jianyou Su, Zijie Tang, Huimin Wang, Shaoqin Ju, and Jianxin Wang. "Establishment of an absolute quantitative method for measurement of urinary cystatin C by stable isotope dilution ultra high performance liquid chromatography tandem mass spectrometry." Analytical Methods 10, no. 43 (2018): 5236–41. http://dx.doi.org/10.1039/c8ay02018c.

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Ferreira, J. A., V. Talamine, J. F. Facco, T. M. Rizzetti, J. M. S. Ferreira, F. A. Oliveira, O. D. Prestes, et al. "Determination of pesticide residues in coconut tree trunks by modified QuEChERS method and ultra-high-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry." Analytical Methods 7, no. 10 (2015): 4237–45. http://dx.doi.org/10.1039/c5ay00323g.

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Konak, Ü. İ., H. A. Yatmaz, Ş. Nilüfer, T. Erkaymaz, and M. Certel. "Multiresidue method for the simultaneous analysis of antibiotics and mycotoxins in feeds by ultra-high performance liquid chromatography coupled to tandem mass spectrometry." Acta Alimentaria 50, no. 1 (March 5, 2021): 74–82. http://dx.doi.org/10.1556/066.2020.00159.

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AbstractResidues in animal feeds and foods of animal origin have been important safety issue concerning both human and animal health. A multiresidue method for determination of eight mycotoxins and ten antibiotics was developed and validated in animal feeds by using QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction followed by UHPLC-MS/MS. Optimisation of UHPLC-MS/MS parameters was performed to achieve good separation and resolution. The method was validated according to the European Commission Decision 2002/657/EC. Matrix matched calibration curves showed good r2 (≥0.995) values, and limit of quantification (LOQ) values varied between 1.2 and 5.2 μg kg−1. Average recoveries ranged from 60 to 102% with relative standard deviations of 2.2 and 15.6% for all type of feed samples except for tetracyclines, lincomycin, tylosin, ochratoxin A, and fumonisin (B1 and B2).

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de Oliveira, Júlia A., Lenise J. P. Izeppi, Roberta F. Loose, Daniela K. Muenchen, Osmar D. Prestes, and Renato Zanella. "A multiclass method for the determination of pharmaceuticals in drinking water by solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry." Analytical Methods 11, no. 17 (2019): 2333–40. http://dx.doi.org/10.1039/c9ay00289h.

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Sun, Yanqin, Xudong Zhu, Xixi Shen, and Wei Wang. "Determination of Carrageenan in Livestock and Poultry Meat by Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry." International Journal of Analytical Chemistry 2021 (September 24, 2021): 1–8. http://dx.doi.org/10.1155/2021/5277453.

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Ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has become the main method for the detection and analysis of food additives because of its good separation, high selectivity, and high sensitivity. The aim of this study was to establish an UHPLC-MS/MS method that can quickly and accurately measure the content of carrageenan in livestock and poultry meat. Chromatographic separation was performed on an ACQUITY UPLC BEH HILIC C18 column (2.1 mm × 50 mm, 1.7 μm) using a gradient elution with methanol and 0.1% (v/v) formic acid in water as a mobile phase. The quantitative analysis was executed using a triple quadrupole mass spectrometer in which electrospray ionization, multiple reaction monitoring, and negative mode were operated. The retention time was about 1.3 min for carrageenan. The carrageenan content showed a good linear relationship from 0.05 to 1.00 g/kg. The limit of detection (LOD) was 0.06 g/kg, and the limit of quantification (LOQ) was 0.18 g/kg. The standards were spiked at three levels (low, medium, and high) and were analyzed in six replicates. The recovery values of carrageenan in pork, beef, lamb, chicken, and duck meat were 82.06–111.55%, 85.43–112.50%, 89.55–116.00%, 83.80–102.15%, and 82.41–110.90%, respectively. The relative standard deviations (RSDs) were all lower than 7.51%. The developed method shows a high recovery rate and good precision and can be used for the rapid detection of carrageenan in livestock and poultry meat.

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De Nicolò, Amedeo, Alice Ianniello, Micol Ferrara, Valeria Avataneo, Jessica Cusato, Miriam Antonucci, Elisa De Vivo, et al. "Validation of a UHPLC-MS/MS Method to Quantify Twelve Antiretroviral Drugs within Peripheral Blood Mononuclear Cells from People Living with HIV." Pharmaceuticals 14, no. 1 (December 25, 2020): 12. http://dx.doi.org/10.3390/ph14010012.

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Recently, anti-HIV treatment has achieved high efficacy and tolerability. Nevertheless, few data are available about the intracellular penetration of antiretrovirals, partly due to the technical challenges related to intracellular quantification. This work aimed to validate an ultra-high performance liquid chromatography (UHPLC) tandem mass spectrometry (MS/MS) method for the simultaneous quantification of maraviroc, nevirapine, rilpivirine, dolutegravir, raltegravir, cobicistat, darunavir, ritonavir, atazanavir, efavirenz, elvitegravir, and etravirine within peripheral blood mononuclear cells (PBMCs) and apply it to samples from patients. PBMCs were isolated by density gradient on cell preparation tubes (CPT). Samples were prepared by addition of internal standards (IS), sonication, centrifugation, and drying. Reconstituted extracts underwent chromatographic separation by reversed phase UHPLC and detection was performed by electrospray ionization and multiple reaction monitoring. Method validation followed FDA and EMA guidelines, showing acceptable accuracy, precision, recovery and IS-normalized matrix effect. The application to 56 samples from patients undergoing antiretroviral treatment provided description of intracellular penetration, showing method eligibility for future studies.

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Xu, Dan, Yang Zhang, Juji Dai, Yongyu Bai, Yuwu Xiao, and Meng-tao Zhou. "A fast, sensitive, and high throughput method for the determination of nintedanib in mouse plasma by UPLC-MS/MS." Analytical Methods 7, no. 16 (2015): 6561–65. http://dx.doi.org/10.1039/c5ay01207d.

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A sensitive and rapid ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed to determine nintedanib in mice plasma using diazepam as the internal standard (IS).

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Wu, Zhijiang, Jinping Liu, and Ying Peng. "QuEChERS purification prior to stable isotope dilution-ultra-high performance liquid chromatography tandem mass spectrometry to determine organophosphate esters of trace amounts in dairy products." Analytical Methods 9, no. 15 (2017): 2290–98. http://dx.doi.org/10.1039/c6ay03162e.

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Barreca, Salvatore, Maddalena Busetto, Luisa Colzani, Laura Clerici, Valeria Marchesi, Laura Tremolada, Daniela Daverio, and Pierluisa Dellavedova. "Hyphenated High Performance Liquid Chromatography–Tandem Mass Spectrometry Techniques for the Determination of Perfluorinated Alkylated Substances in Lombardia Region in Italy, Profile Levels and Assessment: One Year of Monitoring Activities During 2018." Separations 7, no. 1 (March 11, 2020): 17. http://dx.doi.org/10.3390/separations7010017.

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In this research paper, we report a hyphenated technique based on ultra-high performance liquid chromatography–tandem mass spectrometry for the determination of twelve Perfluorinated Alkylated Substances in surface and groundwater samples from Lombardia Region during the monitoring activities in 2018 as new emerging and toxic pollutants. A green analytic method, developed by using an online Solid Phase Extraction coupled with UHPLC-MS/MS and previously validated, was applied for 4992 determinations conducted on 416 samples from 109 different sampling stations. Among the results, PFOS, PFOA, PFBA, PFBS, PFPeA and PFHxA were identified as the most abundant analytes detected. PFASs concentrations, in most cases, were below the limits of quantification and, in the cases where the limits of quantification have been exceeded, the values found were lower than Italy directive. PFOS is an exception and in fact this compound was detected in 76% of analyzed samples (surface and ground waters). Solid phase extraction with high performance liquid chromatography–tandem Mass Spectrometry has proved to be a very good Hyphenated techniques able to detect low concentrations of pollutants in surface and groundwater samples.

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Kao, Chih-Chin, San-Yuan Wang, Yung-Kun Chuang, Wei-Yuan Lee, Wei-Chiao Chang, Mai-Szu Wu, Tai-Chih Kuo, and I.-Lin Tsai. "Clinical Mass Spectrometry Discovered Human IgG Sialylation as a Potential Biosignature for Kidney Function." Journal of Personalized Medicine 11, no. 8 (July 31, 2021): 761. http://dx.doi.org/10.3390/jpm11080761.

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Immunoglobulin G (IgG) N-glycosylation was discovered to have an association with inflammation status, which has the potential to be a novel biomarker for kidney diseases. In this study, we applied an ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method to plasma and urine samples from 57 individuals with different levels of kidney function. Natural abundances of total IgG, IgG1, IgG2, and IgG3 subclasses in plasma showed positive correlations to the estimated glomerular filtration rates (eGFRs). Eighteen IgG glycopeptides also showed positive correlations. In contrast, higher IgG amounts were found in urine samples from participants with lower eGFR values. After normalizing IgG glycopeptides from plasma to their respective protein amounts, H4N4F1S1-IgG1 (r = 0.37, p = 0.0047, significant) and H5N4F1S1-IgG1 (r = 0.25, p = 0.063, marginally significant) were the two glycopeptides that still had positive correlations with eGFRs. The results showed that the UHPLC-MS/MS method is capable of investigating IgG profiles, and monitoring IgG and glycosylation patterns is worthy of further clinical application for kidney disease.

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Li, Xiaowei, Yuebin Ke, Yingyu Wang, Chengfei Wang, Dongyang Ye, Xue Hu, Lan Zhou, and Xi Xia. "Confirmatory Analysis of Nitroimidazoles and Hydroxy Metabolites in Honey by Dispersive-Solid Phase Extraction and Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry." Molecules 23, no. 12 (December 18, 2018): 3350. http://dx.doi.org/10.3390/molecules23123350.

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An ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry (UHPLC-MS/MS) method was developed and validated for confirmatory analysis of four nitroimidazoles and three hydroxy metabolites in honey. Honey samples were dissolved in 2% formic acid solution and nitroimidazoles and metabolites were isolated and enriched by dispersive-solid phase extraction using mixed-mode strong cation-exchange sorbent. The determination involves separation of analytes on an UHPLC C18 column and detection by multiple reaction monitoring in positive ionization mode. The recovery of the method was ranged from 90.2 to 105.6% with inter-day relative standard deviations of less than 11.2%. The limits of detection and limits of quantification were in the ranges of 0.02–0.07 µg/kg and 0.05–0.2 µg/kg, respectively. Honey samples from the market were analyzed to demonstrate the applicability of the proposed method.

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Wang, Tian-Ming, Li-Qin Ding, Jia-Hua Jin, Rong Shi, Jie Zhong, Cui Gao, Qian Wang, Li Zhu, and Yue-Ming Ma. "Simultaneous determination of 14 major components in Longhu Rendan pills by ultra-high-performance liquid chromatography coupled with electrospray ionisation tandem mass spectrometry." Anal. Methods 6, no. 9 (2014): 2923–29. http://dx.doi.org/10.1039/c3ay42152j.

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Wu, Zhijiang, Yansheng Xu, Mianchang Li, Xindong Guo, Yanping Xian, and Hao Dong. "Simultaneous determination of fluorescent whitening agents (FWAs) and photoinitiators (PIs) in food packaging coated paper products by the UPLC-MS/MS method using ESI positive and negative switching modes." Analytical Methods 8, no. 5 (2016): 1052–59. http://dx.doi.org/10.1039/c5ay02414e.

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Malaca, Sara, Francesco Paolo Busardò, Massimo Gottardi, Simona Pichini, and Emilia Marchei. "Dilute and shoot ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS) analysis of psychoactive drugs in oral fluid." Journal of Pharmaceutical and Biomedical Analysis 170 (June 2019): 63–67. http://dx.doi.org/10.1016/j.jpba.2019.02.039.

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He, Dong. "Simultaneous determination of sixteen industrial pollutants in infant formula milk powder by dispersive solid phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry." Analytical Methods 9, no. 17 (2017): 2561–69. http://dx.doi.org/10.1039/c7ay00652g.

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Malaca, Sara, Emilia Marchei, Bernardino Barceló Martín, Adele Minutillo, and Simona Pichini. "Novel fast ultra‐performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) and extraction of ethylglucuronide in meconium samples." Drug Testing and Analysis 11, no. 9 (June 27, 2019): 1471–75. http://dx.doi.org/10.1002/dta.2658.

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Vujovic, Maja, Milan Jokanovic, and Goran Nikolic. "In vitro dissolution profile study of mucolytic drug ambroxol hydrochloride from solid oral dosage form by UHPLC-MS/MS." Chemical Industry 71, no. 1 (2017): 75–83. http://dx.doi.org/10.2298/hemind160315020v.

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In this paper a simplified dissolution test was performed for the release of ambroxol from tablets according to the European Pharmacopoeia. In vitro, three different dissolution media; 0.1 M HCl pH 1.2, acetate buffer (ABS) pH 4.5 and phosphate buffer (PBS) pH 6.8 were used for the simulation of the gastrointestinal conditions at temperature of 37.0?0.5?C. The drug release was evaluated by a new ultra - high performance liquid chromatography (UHPLC) - tandem mass spectrometry (MS/MS) method. The method was validated to meet requirements as per ICH guidelines which include linearity, specificity, precision, accuracy and robustness. The corresponding dissolution profiles showed more than 80% drug release within 30 minutes without significant differences. Further, the developed and validated UHPLC-MS/MS method could find a useful application in the process of production, quality control and bioavailability/bioequivalence studies of new pharmaceutical formulations of drugs in order to achieve a safe therapeutic efficacy.

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Ferrazza Alves Giordani, Camila, Sarah Campanharo, Nathalie Ribeiro Wingert, Lívia Maronesi Bueno, Joanna Wittckind Manoel, Cássia Virginia Garcia, Nadia Maria Volpato, et al. "UPLC-ESI/Q-TOF MS/MS Method for Determination of Vildagliptin and its Organic Impurities." Journal of Chromatographic Science 58, no. 8 (July 24, 2020): 718–25. http://dx.doi.org/10.1093/chromsci/bmaa040.

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Abstract Vildagliptin (VLG) corresponds to a drug used for the treatment of diabetes mellitus. This disease requires continuous treatment, and so the control of impurities present in it is important to assure the quality of this drug. Thus, it is necessary to use sensitive and selective detection techniques and the ultra-performance liquid chromatography is a better option compared with high-performance liquid chromatography because it enhances the separation efficiency with a shorter analysis time and an increased resolution. This research analysis was accomplished by using liquid chromatography/tandem mass spectrometry, and the quantification was performed by using an extracted ion from the VLG drug and its main organic impurities of synthesis. During the validation process, following international standards, the method proved to be linear for the tree substances (R2 = 0.997–0.998) and the analysis of variance showed a non-significant linearity deviation (P > 0.05). Three critical factors were selected to evaluate method robustness with a full factorial experimental design, and the changes in the parameters were found to be not significant for the quantification of VLG and its impurities. The ultra-performance liquid chromatography-tandem mass spectrometry for the determination of impurities in VLG was precise, accurate and robust proving to be effective for analysis in the pharmaceutical industry and to improve the quality, safety and effectiveness of the new drug developed.

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Schusterova, Dana, Jana Hajslova, Vladimir Kocourek, and Jana Pulkrabova. "Pesticide Residues and Their Metabolites in Grapes and Wines from Conventional and Organic Farming System." Foods 10, no. 2 (February 2, 2021): 307. http://dx.doi.org/10.3390/foods10020307.

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In this study, the occurrence of pesticide residues and their metabolites in grapes and wines was investigated. A targeted analysis of 406 pesticide residues in 49 wine and grape samples from organic and conventional production were performed using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction method, followed by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry. Multiple residues (>4 residues/sample) were detected in 22 tested samples. The most commonly detected residues were fungicides (e.g., boscalid) and insecticides (e.g., methoxyfenozide). An ultra-high-performance liquid chromatography–high resolution mass spectrometry method (UHPLC–(HR)MS) was used for screening of pesticide metabolites. We also provide a method and database for detecting pesticide metabolites (extending our previously published database to 49 metabolites originating from 25 pesticides). An introduced strategy of targeted screening of pesticide metabolites was applied for authentication of 27 organic grapes and wines. In total, 23 samples were free of quantifiable residues/detected metabolites or contained residues approved for organic production.

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de Souza, M. P., T. M. Rizzetti, J. Z. Francesquett, O. D. Prestes, and R. Zanella. "Bar adsorptive microextraction (BAμE) with a polymeric sorbent for the determination of emerging contaminants in water samples by ultra-high performance liquid chromatography with tandem mass spectrometry." Analytical Methods 10, no. 7 (2018): 697–705. http://dx.doi.org/10.1039/c7ay02792c.

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Ben Haj Yahia, Imen, Yosr Zaouali, Maria Letizia Ciavatta, Alessia Ligresti, Rym Jaouadi, Mohamed Boussaid, and Adele Cutignano. "Polyphenolic Profiling, Quantitative Assessment and Biological Activities of Tunisian Native Mentha rotundifolia (L.) Huds." Molecules 24, no. 13 (June 26, 2019): 2351. http://dx.doi.org/10.3390/molecules24132351.

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Phenolic profiling of ten plant samples of Mentha rotundifolia (L.) Huds. collected from different bioclimatic areas of Tunisia, was for the first time carried out by using a fast ultra-high-performance liquid chromatography (UHPLC)-high resolution tandem mass spectrometry (HRMS/MS) method on a Q Exactive platform equipped with an electrospray ionization (ESI) source. An intraspecific, interpopulation variability was evidenced and a total of 17 polyphenolic metabolites were identified and quantified by using the UHPLC-HRESIMS/MS method, here validated for specificity, linearity, limit of detection, limit of quantitation, accuracy and precision. The quantitative method resulted sensitive at the nM level and reliable for rapid polyphenol quantification in vegetal matrices. The metabolomic study allowed us to identify a new compound, named salvianolic acid W, which was isolated and characterized mainly by NMR and MS analysis. A statistical correlation of the phenolic composition with antioxidant and anti-acetylcholinesterase activities was provided.

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Gbylik-Sikorska, Małgorzata, Anna Gajda, Ewelina Nowacka-Kozak, Beata Łebkowska-Wieruszewska, and Andrzej Posyniak. "Multi-Class Procedure for Analysis of 50 Antibacterial Compounds in Eggshells Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry." Molecules 26, no. 5 (March 4, 2021): 1373. http://dx.doi.org/10.3390/molecules26051373.

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In this work, for the first time, Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry (UHPLC–MS/MS) method was developed for qualitative and quantitative analysis of veterinary antibiotics (cephalosporins, diaminopyrimidines, fluoro(quinolones), lincosamides, macrolides, penicillins, pleuromutilins, sulfonamides, tetracyclines, and sulfones) in hen eggshells. The sample preparation method is based on a liquid–liquid extraction with a mixture of metaphosphoric acid, ascorbic acid, EDTA disodium salt dihydrate, and acetonitrile. The chromatographic separation was performed on Luna® Omega Polar C18 10 column in gradient elution mode and quantitated in an 8 min run. Validation such as linearity, selectivity, precision, recovery, matrix effect, limit of quantification (LOQ), and limit of detection (LOD) was found to be within the acceptance criteria of the validation guidelines of the Commission Decision 2002/657/EC and EUR 28099 EN. Average recoveries ranged from 81–120%. The calculated LOQ values ranged from 1 to 10 µg/kg, the LOD values ranged from 0.3 to 4.0 µg/kg, depending on analyte. The developed method has been successfully applied to the determination of antibacterial compounds in hen eggshell samples obtained from different sources. The results revealed that enrofloxacin, lincomycin, doxycycline, and oxytetracycline were detected in hen eggshell samples.

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Wang, Bo, Jianyu Liu, Xia Zhao, Kaizhou Xie, Zhixiang Diao, Genxi Zhang, Tao Zhang, and Guojun Dai. "Determination of Eight Coccidiostats in Eggs by Liquid–Liquid Extraction–Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry." Molecules 25, no. 4 (February 22, 2020): 987. http://dx.doi.org/10.3390/molecules25040987.

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A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI+) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs.

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Neuhof, Torsten, Robert Köppen, Matthias Koch, and Irene Nehls. "Letter: High-Performance Liquid Chromatography/Electrospray Mass Spectrometry Analysis of the Mycotoxin Aurofusarin." European Journal of Mass Spectrometry 14, no. 5 (April 1, 2008): 329–33. http://dx.doi.org/10.1255/ejms.935.

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High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) can be used for simultaneous quantification of various mycotoxins in contaminated food samples. Therefore, multi-mycotoxin methods have been developed in the last couple of years. To enlarge these methods for further analytes, we have developed a LC-MS/MS method for the quantification of the mycotoxin aurofusarin. Additionally, further LC-MS n experiments were performed to demonstrate the fragmentation pattern of aurofusarin. Applicable multiple reaction monitoring (MRM) transitions of aurofusarin were found and optimized by parameter variation of the tandem mass spectrometer. The applicability of the developed method was tested by analysis of naturally contaminated wheat.

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Han, Jianwei, Wenbo Zhu, Ling Yu, Yajun Chen, Gaosong Wu, and Zhibin Wang. "Simultaneous determination and pharmacokinetics studies of five isoflavones in rat plasma by UHPLC-MS/MS after oral administration of Radix Astragali extract." Acta Chromatographica 34, no. 1 (September 1, 2021): 24–31. http://dx.doi.org/10.1556/1326.2020.00845.

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Abstract A rapid, sensitive and convenient method based on ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was developed and validated for the simultaneous quantification of calycosin-7-O-β-d-glucoside (CCSG), ononin, calycosin, (6aR,11aR)-9,10-dimethoxypterocarpan-3-O-β-d-glucopyanoside (DPPG), and 7,2′-dihydroxy-3′,4′-dimethoxyisoflavan-7-O-β-d-glucopyanoside (DIFG) in rat plasma after oral administration of the methanol extraction from Radix Astragali. Theophylline played the role of internal standard (IS). Preparation of plasma samples by liquid-liquid extraction method with ethyl acetate after precipitation of protein with methanol. The analytes were detected with a triple quadrupole tandem mass spectrometery (MS) in multiple reaction monitoring (MRM) mode and a positive ion electrospray ionization (ESI). The method was validated with the concentration ranges of 1.96–62.69 ng/mL for CCSG, 1.70–54.5 ng/mL for ononin, 1.85–59.06 ng/mL for calycosin, 2.14–137.24 ng/mL for DPPG and1.96–125.25 ng/mL for DIFG, respectively. The method had the lower limit of quantification (LLOQ) with 0.49, 0.21, 0.92, 1.07, and 0.98 ng/mL for CCSG, ononin, calycosin, DPPG and DIFG respectively, and the precision less than 10%. The RSD of the accuracy was in the range of −4.35–8.91%. The results may be helpful to provide more accurate references to clinical application of this herb.

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Lin, Chao-Zhan, Run-Jing Zhang, Yu-Feng Yao, Xiao-Dan Huang, Rong-Bo Zheng, Bo-Jian Wu, and Chen-Chen Zhu. "Qualitative and Quantitative Analysis of the Major Constituents in WLJ Herbal Tea Using Multiple Chromatographic Techniques." Molecules 23, no. 10 (October 12, 2018): 2623. http://dx.doi.org/10.3390/molecules23102623.

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Quality control of Chinese herbal tea remains a challenge due to our poor knowledge of their complex chemical profile. This study aims to investigate the chemical composition of one of the best-selling and famous brand of beverage in China, Wanglaoji Herbal Tea (WLJHT), via a full component quantitative analysis. In this paper, a total of thirty-two representative constituents were identified or tentatively characterized using ultra-high performance liquid chromatography coupled with quadrupole tandem time-of-flight mass spectrometry (UPLC-Q-TOF-MS). Moreover, the quantitative analyses of fourteen constituents were performed by high performance liquid chromatography with a triple quadruple tandem mass spectrometry (HPLC-MS/MS) method and saccharide compositions of WLJHT were also quantitatively determined by high performance liquid chromatography (HPLC) with evaporative light scattering detector (ELSD) on a Hilic column, separately. Using multiple chromatographic techniques presented a good precision, sensitivity, repeatability and stability, and was successfully applied to analyze 16 batches of WLJHT samples. Therefore, it would be a reliable and useful approach for the quality control of WLJHT.

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Liu, Chu, Yinghe Ji, Xu Jiang, Xucan Yuan, Xinyue Zhang, and Longshan Zhao. "The determination of pesticides in tea samples followed by magnetic multiwalled carbon nanotube-based magnetic solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry." New Journal of Chemistry 43, no. 14 (2019): 5395–403. http://dx.doi.org/10.1039/c8nj06536e.

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A simple and efficient method regarding ultrasound-assisted extraction combined with magnetic solid-phase extraction (UA-MSPE) by UHPLC-MS/MS was set up for the determination of three pesticides in tea leaf samples.

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Lin, Senyu, Yanping Xian, Zhiqing Xun, Siyan Li, Xinjia Liu, Weifeng Du, Jinfeng Huang, Xindong Guo, and Hao Dong. "Solid-phase extraction coupled with ultra performance liquid chromatography tandem mass spectrometry to determine seven halogenated salicylanilides in cosmetics." RSC Advances 6, no. 54 (2016): 49011–18. http://dx.doi.org/10.1039/c6ra07944j.

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A solid-phase extraction (SPE) purification coupled with ultra performance liquid chromatography tandem mass spectrometry (SPE-UPLC-MS/MS) method was developed for simultaneous determination of seven halogenated salicylanilides in cosmetics.

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Martin, Frederic, Catherine Gimenez, Patric Fontannaz, Tamara Kilinc, Esther Campos-Giménez, and Dawn Dowell. "Choline in Infant Formula and Adult/Pediatric Nutritional Formula by Ultra High-Performance Liquid Chromatography/Tandem Mass Spectrometry: AOAC First Action 2012.18." Journal of AOAC INTERNATIONAL 96, no. 6 (November 1, 2013): 1396–99. http://dx.doi.org/10.5740/jaoacint.13-195.

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Abstract The method described below is for the determination of choline in infant formula and adult/pediatric nutritional formula by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The single-laboratory validation data were submitted to the Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Expert Review Panel (ERP) for review at the AOAC INTERNATIONAL Annual Meeting held September 30 to October 3, 2012 in Las Vegas, NV. The ERP determined that the data reviewed met the standard method performance requirements set by SPIFAN, and the method was approved as AOAC Official First Action. The analytical range was found to be between 0.16 and 3.2 μg/mL. The recovery rates were within 80–120% at 50 and 100% of native levels for all samples. Repeatability precision (RSDr) was <3%, with intermediate reproducibility (RSDir) no higher than 4%.

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Journal articles on the topic 'Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry (UHPLC-MS/MS)'

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