scholarly journals Multiresidue Analysis of Pesticides in Soil by High-Performance Liquid Chromatography with Tandem Mass Spectrometry

2009 ◽  
Vol 92 (5) ◽  
pp. 1566-1575 ◽  
Author(s):  
José Fenoll ◽  
Pilar Hellín ◽  
Carmen M Martnez ◽  
Pilar Flores
Keyword(s):  
High Performance ◽  
Single Phase ◽  
Multiple Reaction Monitoring ◽  
Soil Samples ◽  
Reaction Monitoring ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Multiresidue Analysis ◽  
Multiple Reaction Monitoring Mode

Abstract An analytical multiresidue method using HPLC/MS/MS with a triple-quadrupole mass spectrometer in the multiple reaction monitoring mode for the simultaneous determination of 54 pesticides in soil has been developed. The procedure involved initial single-phase extraction of soil sample with acetonitrile by sonication, followed by liquidliquid partitioning after addition of NaCl. The average recovery by the HPLC/MS/MS method obtained for these compounds varied from 63.2 to 113.8, with an RSD between 1.9 and 7.1. The method gave good linearity over the assay range of 10500 g/L (except famoxadone, 501000 g/L); the LOD and LOQ for the pesticides varied from 0.02 to 13.2 and from 0.1 to 43.9 g/kg, respectively. The proposed method was used to determine pesticide levels in soil samples from two experimental vineyards and two tomato greenhouses.

scholarly journals UHPLC-QQQ-MS/MS assay for quantification of dianthrones as potential toxic markers of Polygonum multiflorum Thunb: Application to the standardization of TCMs with endogenous toxicity

2021 ◽  
Author(s):  
Jian-Bo Yang ◽  
Yun-Fei Song ◽  
Yue Liu ◽  
Hui-Yu Gao ◽  
Qi Wang ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Triple Quadrupole ◽  
Quadrupole Mass ◽  
Polygonum Multiflorum ◽  
Triple Quadrupole Mass Spectrometer ◽  
Benefit Risk Assessment ◽  
Heparg Cells

Abstract Background: The raw and processed roots of Polygonum multiflorum Thunb (PM) are commonly used in clinical practice to treat diverse diseases; however, the reports of hepatotoxicity induced by Polygoni Multiflori Radix (PMR) and Polygoni Multiflori Radix Praeparata (PMRP) have emerged worldwide. Thus, it is necessary for researcher to explore the methods to improve its quality standards and further ensure its quality and treatment effect.Methods: In the present study, an ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QQQ- MS/MS) method has been optimized and validated for the determination of dianthrones in PMR and PMRP, using bianthronyl as the internal standard. Chromatographic separation with a gradient mobile phase (A: acetonitrile and B: water containing 0.1% formic acid (v/v)) at a flow rate of 0.25 mL/min was achieved on a Waters Acquilty UPLC BEH b) C18 column (2.1 mm × 50 mm, 1.7 µm). A triple quadrupole mass spectrometer (TQMS) was operated in negative ionization mode with multiple reaction monitoring for the quantitative analysis of six dianthrones. Meanwhile, compounds 5 and 6 were further evaluated for cytotoxicity of HepaRG cells by CCK8 assay.Results: The UHPLC-QQQ-MS/MS method was first developed to simultaneous determination of six dianthrones in PMR and PMRP, namely polygonumnolides C1–C4 (1–4), trans-emodin dianthrones (5), and cis-emodin dianthrones (6). The contents of 1~6 in 90 batches of PMR were in the range of 0.027-19.04, 0.022-13.86, 0.073 -15.53, 0.034 -23.35, 0.38-83.67 and 0.29 -67.00 µg/g, respectively. The contents of 1~6 in 86 batches of commercial PMRP were in the range of 0.020-13.03, 0.051-8.94, 0.022-7.23, 0.030 -12.75, 0.098-28.54 and 0.14-27.79 µg/g, respectively. The six dianthrones were almost completely gone after reasonable processing for 24 h. Meanwhile, compounds 5 and 6 showed the inhibitory activity against HepaRG cells with the IC50 values of 10.98 and 15.45 μM, respectively. Furthermore, a systematic five-step strategy to realize the standardization of TCMs with endogenous toxicity is proposed for the first time, involving the establishment of determination methods, determination of the toxic markers, the standardization of processing method, the development of limit standards and benefit-risk assessment.Conclusion: The results of cytotoxicity evaluation of dianthrone indicated that trans-emodin dianthrones (5) and cis-emodin dianthrones (6) could be selected as the toxic markers of PMRP. Taking PMR and PMRP for example, we hope this study provided insight into the standardization and internationalization of endogenous toxic TCMs, with the main purpose of improving public health by scientifically using TCMs to treat diverse complex diseases in future.

scholarly journals Determination of Anlotinib, a Tyrosine Kinase Inhibitor, in Rat Plasma by UHPLC-MS/MS and Its Application to a Pharmacokinetic Study

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Zhe Wang ◽  
Le-jing Lian ◽  
Yan-yan Dong ◽  
Xiao Cui ◽  
Jian-chang Qian ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Kinase Inhibitor ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Reaction Monitoring ◽  
Receptor Kinase ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer

Anlotinib is a novel inhibitor of receptor kinase tyrosine with multitargets and has a broad spectrum of inhibitory action on tumor angiogenesis and growth. A simple and rapid UHPLC-MS/MS bioanalytical method was validated for the determination of anlotinib in rat plasma, using imatinib as an internal standard. An Acquity BEH C18 column was used to separate analytes. The eluents consisted of formic acid/water (0.1 : 100, v/v) and acetonitrile with a mobile phase. A triple quadrupole mass spectrometer was operated for the quantification with multiple reaction monitoring (MRM) to determine transitions: 408.2 ⟶ 339.1 for anlotinib, and 494.3 ⟶ 394.1 for imatinib. The validated range was 0.1–50 ng/mL for anlotinib. Mean recovery rate of anlotinib in plasma was ≥99.32% and reproducible. Also, the intra- and interday precisions were both below 15%. This robust method was successfully applied to support the pharmacokinetic study of anlotinib in rats.

scholarly journals Fingerprint and multi-component quantitative analyses for quality evaluation of Rhizoma coptidis steamed with rice wine

2021 ◽  
Vol 18 (6) ◽  
pp. 1297-1303
Author(s):  
Jin Wang ◽  
Hai-rong Zeng ◽  
Guan-hua Lou ◽  
Chang-jiang Hu ◽  
Qin-wan Huang ◽  
...  
Keyword(s):  
High Performance ◽  
Quality Evaluation ◽  
Multiple Reaction Monitoring ◽  
Reaction Monitoring ◽  
Rice Wine ◽  
Rhizoma Coptidis ◽  
Relative Standard ◽  
Multiple Reaction Monitoring Mode ◽  
Quantitative Analyses

Purpose: To establish a method for the simultaneous determination of multi-components of Rhizoma coptidis steamed with rice wine (RCRW), and to provide a reference for assessing its standard of quality. Method: Chromatographic separation was performed on a high performance liquid chromatography (HPLC) system to determine the characteristic fingerprint of RCRW. The mobile phase consisted of acetonitrile (A) and 0.1 % trifluoroacetic acid (B), with gradients of B as follows: 15 - 20 % from 0 – 30 min; 20 - 25 % from 30 - 50 min; 25 - 35 % for 50 - 60 min, and 35 % for 60 - 70 min. Results: In the multiple reaction monitoring mode, eight components of RCRW were isolated by HPLCphoto-diode array (PDA) method. A fingerprint of the RCRW was established and 8 peaks were calibrated. The method was further validated in terms of linearity (R2 > 0.9993), precision (relative standard deviation, RSD < 1.51 %); repeatability (RSD < 2.98 %) and stability (RSD < 1.93 %). Mean recovery rate ranged from 96.2 to 103.8 %, while RSD values ranged from 0.92 to 2.88 %. Conclusion: These results show that HPLC-PDA method is accurate and feasible, and that they provide a reference for further comprehensive and effective quality control of RCRW.

scholarly journals Simultaneous Quantification and Pharmacokinetic Study of Five Homologs of Dalbavancin in Rat Plasma Using UHPLC-MS/MS

Molecules ◽  
2020 ◽  
Vol 25 (18) ◽  
pp. 4100
Author(s):  
Difeng Zhu ◽  
Li Ping ◽  
Yawen Hong ◽  
Jiale Shen ◽  
Qinjie Weng ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Pharmacokinetic Analysis ◽  
Pharmacokinetic Studies ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode

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.

Step-by-step real time monitoring of a catalytic amination reaction

2019 ◽  
Vol 55 (78) ◽  
pp. 11727-11730 ◽  
Author(s):  
Gilian T. Thomas ◽  
Eric Janusson ◽  
Harmen S. Zijlstra ◽  
J. Scott McIndoe
Keyword(s):  
Real Time ◽  
Multiple Reaction Monitoring ◽  
Reaction Monitoring ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Amination Reaction ◽  
Catalytic Amination ◽  
Multiple Reaction Monitoring Mode ◽  
Sequential Addition ◽  
The Individual

The multiple reaction monitoring mode of a triple quadrupole mass spectrometer is used to examine the Buchwald–Hartwig amination reaction in real-time using sequential addition of reagents to probe the individual steps in the cycle.

scholarly journals Determination of Polypeptide Antibiotic Residues in Food of Animal Origin by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3261
Author(s):  
Tomasz Bladek ◽  
Iwona Szymanek-Bany ◽  
Andrzej Posyniak
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Animal Origin ◽  
Antibiotic Residues ◽  
Triple Quadrupole Mass Spectrometer ◽  
Limit Of Quantification ◽  
Food Of Animal Origin ◽  
Polypeptide Antibiotic

A novel UHPLC-MS/MS method for the determination of polypeptide antibiotic residues in animal muscle, milk, and eggs was developed and validated. Bacitracin A, colistin A, colistin B, polymyxin B1, and polymyxin B2 were extracted from the samples with a mixture of acetonitrile/water/ammonia solution 25%, 80/10/10 (v/v/v), and put through further evaporation, reconstitution, and filtration steps. The chromatographic separation was performed on a C18 column in gradient elution mode. Mass spectral acquisitions were performed in selective multiple reaction monitoring mode by a triple quadrupole mass spectrometer. The method was validated according to the criteria of Commission Decision 2002/657/EC. The method quantifies polypeptides in a linear range from 10 to 1000 μg kg−1, where the lowest concentration on the calibration curve refers to the limit of quantification (LOQ). The recoveries ranged from 70 to 99%, the repeatability was below 13%, and within-laboratory reproducibility was lower than 15%. The decision limit (CCα) and detection capability (CCβ) values were calculated, and ruggedness and stability studies were performed, to fulfill the criteria for confirmatory methods. Moreover, the developed method may also be used for screening purposes by its labor efficiency.

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