PMID- 37712545 OWN - NLM STAT- MEDLINE DCOM- 20230918 LR - 20230921 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 41 IP - 9 DP - 2023 Sep TI - [Determination of 10 carbamate pesticide residues in liquid milk by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction purification]. PG - 807-813 LID - 10.3724/SP.J.1123.2023.03017 [doi] AB - Carbamates are used in broad-spectrum insecticides and herbicides, and have highly efficient, low-residue, and long-lasting characteristics. However, this type of pesticide exerts mutagenic, teratogenic, carcinogenic, and other adverse effects, and its frequent use can exceed the recommended scope and limits. Research on the determination of carbamate pesticides mainly focuses on foods of plant origin and pays less attention to foods of animal origin. The methods for carbamate determination described in the current national standards have complicated operating procedures and low efficiency. Therefore, highly efficient and accurate methods for carbamate detection in milk must be established. In this work, a rapid method based on pass-through solid-phase extraction (SPE) purification coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 10 carbamate pesticides in liquid milk. The pretreatment and instrument methods were systematically optimized. The milk sample was extracted with acetonitrile, and then purified using a Captiva EMR-Lipid filtration kit. The purified extract was separated on an ACQUITY UPLC BEH C(18) column with mobile phase of methanol and 0.1% formic acid aqueous solution in gradient elution. The flow rate was 0.3 mL/min. Column temperature was 35 ℃. Quantitative analysis was performed using the external standard method with matrix matching curves. The 10 carbamate pesticides showed good linear relationships in the mass concentration range of 2-200 mug/L, with correlation coefficients greater than 0.999. The limits of detection (LODs) and quantification (LOQs) for the 10 carbamate pesticides were 0.045-0.23 and 0.15-0.77 mug/kg, respectively. Recovery tests were conducted using the blank-matrix method at three spiked levels of 15, 50, and 100 mug/kg, and good recoveries for the 10 carbamate pesticides were obtained. In particular, the recoveries for the three spiked levels of 15, 50, and 100 mug/kg were 68.7%-93.3% with relative standard deviations (RSDs) of 1.8%-8.0%. The proposed method is efficient, convenient, accurate, and suitable for the rapid detection of the 10 carbamate pesticides in liquid milk. Compared with the conventional NH(2) and ENVI(TM)-18 SPE columns used in the national standard determination method, the proposed method demonstrated better purification effects. The recoveries for aldicarb sulfoxide, aldicarb sulfone, methomyl, and carbaryl after purification using the Captiva EMR-Lipid kit increased from 60% to 80%. Thus, the proposed method is suitable for targets with strong polarity and gives measurement results with good repeatability and accuracy. FAU - Yue, Chao AU - Yue C AD - Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China. FAU - Zhao, Chao-Qun AU - Zhao CQ AD - Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China. FAU - Mao, Si-Hao AU - Mao SH AD - Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China. FAU - Wang, Zhan-Hua AU - Wang ZH AD - Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China. FAU - Shi, Bei AU - Shi B AD - Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China. FAU - Xu, Xin-Feng AU - Xu XF AD - Zhejiang Chinese Medical University, Hangzhou 310056, China. FAU - Liang, Jing-Jing AU - Liang JJ AD - Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China. LA - chi PT - English Abstract PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Pesticide Residues) RN - 0 (Carbamates) RN - 0 (Pesticides) RN - 0 (Lipids) SB - IM MH - Animals MH - *Pesticide Residues MH - Carbamates MH - Milk MH - Chromatography, Liquid MH - Tandem Mass Spectrometry MH - *Pesticides MH - Lipids PMC - PMC10507527 OTO - NOTNLM OT - carbamate pesticide OT - enhanced matrix removal-lipid cleaning OT - liquid milk OT - pass-through solid-phase extraction purification OT - ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) EDAT- 2023/09/15 12:45 MHDA- 2023/09/18 12:42 PMCR- 2023/09/08 CRDT- 2023/09/15 07:32 PHST- 2023/09/18 12:42 [medline] PHST- 2023/09/15 12:45 [pubmed] PHST- 2023/09/15 07:32 [entrez] PHST- 2023/09/08 00:00 [pmc-release] AID - 10.3724/SP.J.1123.2023.03017 [doi] PST - ppublish SO - Se Pu. 2023 Sep;41(9):807-813. doi: 10.3724/SP.J.1123.2023.03017.