Simultaneous Determination of 27 Pesticides in Ginseng by UPLC/MS/MS and Modified QuEChERS Procedure

2015 ◽  
Vol 98 (3) ◽  
pp. 839-846 ◽  
Author(s):  
Ruoxin Wu ◽  
Qiyong Chen ◽  
Shujing Li ◽  
Guoliang Fan
Keyword(s):  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Safe Procedure ◽  
Reaction Monitoring ◽  
Modified Quechers ◽  
Polarity Switching ◽  
Multiple Reaction Monitoring Mode ◽  
Primary Secondary Amine ◽  
Ionization Mode

Abstract A novel, simple, and rapid method for the quantification of 27 commonly used pesticides in ginseng incorporating a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was developed and validated. The pesticides were extracted with 1% acetic acid in acetonitrile and extracts purified by use of the mixed sorbents primary-secondary amine, C18, and graphitized carbon black. Quantitative analysis of all pesticides was performed by ultra-performance LC/MS/MS in the positive ionization mode in a single run due to the fast polarity switching capability of the mass spectrometer. Two precursor-product ion transitions were monitored for each compound in the multiple reaction monitoring mode. Quantification was carried out using matrix-matched standards for calibration. Recoveries of the proposed method from the spiked samples were achieved in the range 62.8–108.5%, and RSD ranged from 1.5 to 11.8%.

Simultaneous Determination of 44 Pesticides in Tobacco by UPLC/MS/MS and a Modified QuEChERS Procedure

2013 ◽  
Vol 96 (2) ◽  
pp. 422-431 ◽  
Author(s):  
Xuyan Chen ◽  
Kongxiang Zhao ◽  
Baokun Ge ◽  
Qiyong Chen
Keyword(s):  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Modified Quechers ◽  
Negative Ionization Mode ◽  
Multiple Reaction Monitoring Mode ◽  
Primary Secondary Amine ◽  
Standard Calibration ◽  
Ionization Mode ◽  
Negative Ionization

Abstract A novel, simple, and rapid method for determination of the residues of 44 commonly used pesticides in tobacco was developed based on modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedures. The pesticides were extracted with acetonitrile and purified on a mixed sorbents column of primary secondary amine, C18, and graphitized carbon black. Quantitative determination of all pesticides was performed by ultra-performance LC/MS/MS in the positive or negative ionization mode by a single run due to the fast polarity switching capability of the mass spectrometer. Two precursor-product ion transitions were monitored for each compound in the multiple reaction monitoring mode. Quantification was carried out using matrix-matched standard calibration. The method has been validated by various tobacco cultivars, such as Burley, Oriental, and Virginia from different countries. Recoveries of the proposed method for spiked samples ranged from 71.1 to 109.8%, and RSD values were below 10%. The LOQ values were are all below the guidance residue levels proposed by the Agrochemical Advisory Committee of Cooperation Center for Scientific Research Relative to Tobacco. This method is valuable for measurement of pesticide residues in tobacco for QC and monitoring.

Determination of Dufulin Residue in Vegetables, Rice, and Tobacco Using Liquid Chromatography with Tandem Mass Spectrometry

2015 ◽  
Vol 98 (6) ◽  
pp. 1739-1744 ◽  
Author(s):  
Yanjiao Li ◽  
Ping Lu ◽  
Deyu Hu ◽  
Pinaki S Bhadury ◽  
Yuping Zhang ◽  
...  
Keyword(s):  
Multiple Reaction Monitoring ◽  
Antiviral Agent ◽  
Graphitized Carbon Black ◽  
The Novel ◽  
Multiple Reaction Monitoring Mode ◽  
Primary Secondary Amine ◽  
Rice Samples ◽  
Dispersive Spe ◽  
Actual Trial

Abstract A rapid and accurate LC/MS/MS method using positive electrospray ionization was established for the determination of residues of the novel plant antiviral agent dufulin in samples of tobacco leaf (dry), tomato, cucumber, and rice. Samples were extracted with acetonitrile; cleaned up by dispersive SPE using primary secondary amine, C18, and graphitized carbon black sorbents; separated on a C18 column; and confirmed by multiple reaction monitoring mode MS with a matrix effect of –21.5–19.6%. The method showed satisfactory linearity (R2 ≥0.9912) for the target compound. The LOD and the LOQ were 0.05 and 0.15 μg/kg, respectively. The mean recoveries from four matrixes varied from 71.9 to 93.6% with intraday RSD in the range of 2.9 to 9.0% and interday RSD 6.9 to 15.2%. The method was successfully applied for analysis of dufulin in actual trial samples.

Determination of doravirine in human plasma using liquid–liquid extraction and HPLC–MS/MS

Bioanalysis ◽  
2019 ◽  
Vol 11 (16) ◽  
pp. 1495-1508
Author(s):  
Rajesh Desai ◽  
Brad Roadcap ◽  
Dina Goykhman ◽  
Eric Woolf
Keyword(s):  
Human Plasma ◽  
Dynamic Range ◽  
Multiple Reaction Monitoring ◽  
Development Program ◽  
Liquid Extraction ◽  
Clinical Development Program ◽  
Liquid Liquid Extraction ◽  
Multiple Reaction Monitoring Mode ◽  
Ionization Mode

Aim: A method to quantitate doravirine (MK-1439) in human plasma has been developed to support human clinical trials designed to evaluate the safety, pharmacokinetics and efficacy of the compound. Methodology & results: The analyte was extracted using liquid–liquid extraction, separated on a reverse phase HPLC column, and detected on an API-4000 mass spectrometer using a Turbo-Ion spray source in positive ionization mode coupled with multiple reaction monitoring mode was used for quantification. The dynamic range for the assay was 0.02–10 ng/ml using 100 μl of human plasma. Conclusion: The assay was found to be sensitive, selective and reproducible and applied to support the doravirine clinical development program.

scholarly journals High-Throughput LC/MS/MS Analysis of Ruscogenin and Neoruscogenin in Ruscus aculeatus L.

2009 ◽  
Vol 92 (4) ◽  
pp. 1055-1059 ◽  
Author(s):  
Laurian Vlase ◽  
Béla Kiss ◽  
Georgeta Balica ◽  
Mircea Tas ◽  
Gianina Crisan ◽  
...  
Keyword(s):  
Electrospray Ionization ◽  
Mass Spectrometer ◽  
High Throughput ◽  
Ion Trap ◽  
Multiple Reaction Monitoring ◽  
Reaction Monitoring ◽  
Ionization Source ◽  
Ion Trap Mass Spectrometer ◽  
Multiple Reaction Monitoring Mode ◽  
Ionization Mode

Abstract A new, sensitive LC/MS/MS method was developed for the quantification of ruscogenin and neoruscogenin in hydrolyzed extracts from Ruscus aculeatus L. (Liliaceae). The two sapogenins were separated on a Zorbax SB-C18 column under isocratic conditions. The detection was performed in the multiple reaction monitoring mode using an ion trap mass spectrometer with an electrospray ionization source operated in positive ionization mode. For the quantification of the ruscogenin and neoruscogenin, calibration curves were constructed over the range of 21000 ng/mL. This is the first reported LC/MS/MS method for the simultaneous analysis of ruscogenin and neoruscogenin, and it showed superior sensitivity when compared with other assays described in the literature. The method has been successfully applied to quantify the two sapogenins in aerial (phylloclades) and underground parts (rhizomes, roots) of Ruscus aculeatus L.

A Sensitive LC–MS/MS Method for the Determination of Afatinib in Human Plasma and Its Application to a Bioequivalence Study

2021 ◽  
Author(s):  
Xi Luo ◽  
Xiu Jin Zhang ◽  
Wen Ling Zhu ◽  
Jin Ling Yi ◽  
Wen Gang Xiong ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Ionization Mode

Abstract A high performance liquid chromatography–tandem mass spectrometry assay for the determination of afatinib (AFT) in human plasma was established. A simple sample preparation of protein precipitation was used and separation was achieved on a C18 column by the gradient mixture of mobile Phase A of water (containing 0.1% ammonia) and the mobile Phase B of acetonitrile and water (V:V = 95:5, containing 0.2% ammonia). The multiple reaction monitoring mode was used to monitor the precursor-to-production transitions of m/z 486.2 → m/z 371.4 for AFT and m/z 492.2 → m/z 371.3 for AFT-d6 (internal standard) at positive ionization mode. The calibration curve ranged from 0.100 to 25.0 ng·mL−1 and the correlation coefficient was greater than 0.99. The intra- and inter-batch precision was less than or equal to 10.0%. Accuracy determined at four concentrations was in the range of 92.3–103.3%. In summary, our method was sensitive, simple and reliable for the quantification of AFT and was successfully applied to a bioequivalence study.

scholarly journals Validation of a Method for the Determination of Chloramphenicol in Poultry and Swine Liver by Ultra-Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

2010 ◽  
Vol 93 (5) ◽  
pp. 1666-1671 ◽  
Author(s):  
Xi Xia ◽  
Xiaowei Li ◽  
Shuangyang Ding ◽  
Jianzhong Shen
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Reaction Monitoring ◽  
Polymeric Sorbent ◽  
Multiple Reaction Monitoring Mode ◽  
Swine Liver

Abstract A sensitive and reliable method has been developed and validated for the determination of chloramphenicol in poultry and swine liver using SPE and ultra-performance liquid chromatography (UPLC)/MS/MS. The liver samples were extracted with ethyl acetate, defatted with n-hexane, and further cleaned up using SPE cartridges with polymeric sorbent. An Acquity BEH C18 column was used for gradient UPLC separation, with water and acetonitrile as the mobile phase. The multiple reaction monitoring mode was used for two precursor-product ion transitions for chloramphenicol and one for the internal standard. The method was validated at 0.1, 0.3, and 1.0 µg/kg. Mean recoveries from fortified samples ranged from 95.5 to 106.7% with an RSD of 12.2%. The method LOD was <0.02 µg/kg.

scholarly journals Validation of Multiresidue Method for Analysis of 31 Pesticides in Rice Using Gas Chromatography-Tandem Mass Spectrometry

2017 ◽  
Vol 100 (4) ◽  
pp. 1094-1101 ◽  
Author(s):  
Rahul Mondal ◽  
Ramen Kumar Kole ◽  
Anjan Bhattacharyya
Keyword(s):  
Multiple Reaction Monitoring ◽  
Tandem Ms ◽  
Tandem Mass ◽  
Reaction Monitoring ◽  
Multiresidue Analysis ◽  
Calibration Standards ◽  
Modified Quechers ◽  
Chromatography Tandem Mass Spectrometry ◽  
Maximum Residue Limits ◽  
Multiple Reaction Monitoring Mode

Abstract Five modified QuEChERS were tested for the multiresidue analysis of 31 pesticides in rice. Rice was spiked with mixture solution of pesticides at 10 ng/g. Method selection was based on the LODs (sensitivity) and recovery tests (accuracy) of the pesticides. Analysis was done in GC-tandem MS in multiple reaction monitoring mode with a total run time of approximately 37 min. The selected method was validated after spiking rice at 20 and 100 ng/g in rice. The performance characteristics of the method impacted for all selected pesticides were acceptable according to the guidelines for method validation (recovery of 70–120% with an RSD of <20% and r2 value of ≥0.99). For rice, matrix effect on the signals of the compounds was corrected by using matrix-matched calibration standards. The LOQs met the requirements of the maximum residue limits for pesticides in rice. The developed method allowed for the simultaneous determination and confirmation of a large number of different groups of pesticides and was fast, simple, inexpensive, and useful for the routine analysis of rice.

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.

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