Validation of a Multiresidue Analysis Method for 379 Pesticides in Human Serum Using Liquid Chromatography-Tandem Mass Spectrometry

被引:57
作者
Shin, Yongho [1 ,2 ]
Lee, Jonghwa [1 ,2 ]
Lee, Jiho [1 ,2 ]
Lee, Junghak [1 ,2 ]
Kim, Eunhye [1 ,2 ]
Liu, Kwang-Hyeon [3 ,4 ]
Lee, Hye Suk [5 ]
Kim, Jeong-Han [1 ,2 ]
机构
[1] Seoul Natl Univ, Dept Agr Biotechnol, Seoul 08826, South Korea
[2] Seoul Natl Univ, Res Inst Agr & Life Sci, Seoul 08826, South Korea
[3] Kyungpook Natl Univ, Coll Pharm, Plus KNU Multiomics Based Creat Drug Res Tea BK21, Daegu 41566, South Korea
[4] Kyungpook Natl Univ, Res Inst Pharmaceut Sci, Daegu 41566, South Korea
[5] Catholic Univ Korea, Coll Pharm, Bucheon Si 14662, Gyeonggi Do, South Korea
基金
新加坡国家研究基金会;
关键词
pesticide; multiresidue; intoxication; serum; QuEChERS; LC-MS/MS; QUECHERS SAMPLE PREPARATION; GAS-CHROMATOGRAPHY; ORGANOCHLORINE PESTICIDES; WHOLE-BLOOD; ORGANOPHOSPHORUS PESTICIDES; POLYCHLORINATED-BIPHENYLS; RAPID-DETERMINATION; RESIDUES; EXTRACTION; URINE;
D O I
10.1021/acs.jafc.8b00094
中图分类号
S [农业科学];
学科分类号
09 ;
摘要
A screening method for simultaneous analysis of 379 pesticides in human serum was developed using liquid chromatography tandem mass spectrometry (LC-MS/MS). Electrospray ionization with positive/negative switching mode of LC-MS/MS was adopted, and scheduled multiple reaction monitoring for each target compound was established. The limit of quantitation was 10 ng/mL for 94.5% of the total pesticides, and the correlation coefficients of calibration were >= 0.990 for 93.9% of the pesticides. For the sample preparation, scaled-down QuEChERS were used. Serum (100 mu L) was extracted with acetonitrile (400 mu L), partitioned with magnesium sulfate (40 mg) and sodium chloride (10 mg), and the upper layer was used for analysis without further deanup steps. For the accuracy and precision tests, most of the pesticides showed excellent results in intra- and interday conditions. In the recovery tests at 10, 50, and 250 ng/mL, 85.8-91.8% of all target compounds satisfied the recovery range of 70-120% (relative standard deviation <= 20%).
引用
收藏
页码:3550 / 3560
页数:11
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