PMID- 34227311 OWN - NLM STAT- MEDLINE DCOM- 20210722 LR - 20230916 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 39 IP - 3 DP - 2021 Mar TI - [Rapid screening and confirmation of 415 pesticide residues in red cabbages by liquid chromatography-quadrupole-time of flight-mass spectrometry]. PG - 301-315 LID - 10.3724/SP.J.1123.2020.05006 [doi] AB - An analytical method for the simultaneous rapid screening and accurate confirmation of 415 pesticide residues in red cabbages was established using liquid chromatography-quadrupole-time of flight-mass spectrometry (LC-QTOF/MS) with single acquisition. In the established method, the pesticides in red cabbage were extracted using acetonitrile-acetic acid (99ratio1, v/v) and salted-out using anhydrous magnesium sulfate and sodium chloride. The resultant solution was then cleaned-up by automatic solid phase extraction using a Carbon/NH(2) cartridge. The SPE cartridge was activated with 4 mL acetonitrile-toluene (3ratio1, v/v) and the effluents were discarded. The resultant solution was transferred to the Carbon/NH(2) cartridge, using 3x2 mL acetonitrile-toluene (3ratio1, v/v) to wash the test sample concentrate bottle, and waited until the surface of the test sample concentrate liquid reached the top layer of anhydrous Na(2)SO(4) before transferring the washing liquid to the cartridge. A 30-mL reservoir was attached to the upper part of the SPE cartridge and 25 mL acetonitrile-toluene (3ratio1, v/v) was used to wash the SPE cartridge again. The eluent was evaporated in the glass tube in a water bath at 37 ℃ and shaking speed 150 r/min to reduce the volume to 0.5 mL. Nitrogen was used to dry the concentrates, and the residues were dissolved in 1.0 mL acetonitrile-water (3ratio2, v/v), homogenized by ultrasonication, and passed through 0.22-mum filtering membrane before determination. The dissolved sample solution was loaded onto a ZORBAX SB-C18 column (100 mmx2.1 mm, 3.5 mum) and separated under gradient elution using 0.1% (v/v) formic acid aqueous solution containing 5 mmol/L ammonium acetate and acetonitrile as the binary mobile phase. The eluent from the column was further detected by QTOF/MS under electrospray positive ionization in the MS/MS scanning mode. A matrix-matched external calibration method was used for quantitation. By optimizing the different parameters under Auto MS/MS and All Ions MS/MS acquisition modes, the optimal conditions for All Ions MS/MS under each acquisition mode were obtained, which were then compared for selection of a better mode. The results demonstrated that the developed method can be used to accurately screen and quantify all 415 pesticides in red cabbage. The linear regression correlation coefficients (r(2)) for the 415 pesticides were all greater than 0.990 in the corresponding linear concentration range. In addition, the screening detection limits (SDL) of 411 pesticides were no more than 5 mug/kg, and the limits of quantification (LOQs) of 413 pesticides were no more than 10 mug/kg. At the spiked levels of LOQ, two-fold LOQ, and 10-fold LOQ, the recoveries were in the ranges of 65.7%-118.4%, 72.0%-118.8% and 70.2%-111.2%, with relative standard deviations (RSDs) in the ranges of 0.9%-19.7%, 0.2%-19.9% and 0.6%-19.9%, respectively. The method was applied to detect pesticide residues in the red cabbage samples provided by the 2019 European proficiency test project for unknown pesticide screening (EUPT-SM-11) and accurate quantitation (EUPT-FV-21). For EUPT-SM-11, all the spiked and incurred pesticides in red cabbage were qualified accurately, without false positives or false negatives. This is completely consistent with the final results published by the EU official. For EUPT-FV-21, there were 19 non-volatile pesticides that can be detected by LC-MS, which were then accurately quantitated with the corresponding pesticide standard. The results demonstrate that the proposed method is accurate and reliable. It is also rapid and time-saving, and can be used for high-throughput screening and quantitative determination of pesticide residues in cabbage. It can also be extended to other fruits and vegetable matrices. FAU - Xie, Yujie AU - Xie Y AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. FAU - Chen, Hui AU - Chen H AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. FAU - Ge, Lijuan AU - Ge L AD - Beijing Usi-Star Inspection Technology Co., Ltd., Beijing 100176, China. FAU - Huo, Siyu AU - Huo S AD - Beijing Usi-Star Inspection Technology Co., Ltd., Beijing 100176, China. FAU - Fan, Chunlin AU - Fan C AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. FAU - Lu, Meiling AU - Lu M AD - Agilent Technologies (China) Limited, Beijing 100102, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Pesticide Residues) SB - IM MH - *Brassica/chemistry MH - Chromatography, Liquid MH - *Food Contamination/analysis MH - *Pesticide Residues/analysis MH - Tandem Mass Spectrometry PMC - PMC9403803 OTO - NOTNLM OT - European proficiency test OT - liquid chromatography-quadrupole-time of flight-mass spectrometry (LC-QTOF/MS) OT - pesticide residues OT - red cabbage OT - screening and confirmation EDAT- 2021/07/07 06:00 MHDA- 2021/07/23 06:00 PMCR- 2021/03/08 CRDT- 2021/07/06 07:00 PHST- 2021/07/06 07:00 [entrez] PHST- 2021/07/07 06:00 [pubmed] PHST- 2021/07/23 06:00 [medline] PHST- 2021/03/08 00:00 [pmc-release] AID - 1000-8713-39-3-301 [pii] AID - 10.3724/SP.J.1123.2020.05006 [doi] PST - ppublish SO - Se Pu. 2021 Mar;39(3):301-315. doi: 10.3724/SP.J.1123.2020.05006.