分析测试学报2024，Vol.43Issue(5)：738-745,8.DOI:10.12452/j.fxcsxb.23121149
分散液液微萃取/超高效液相色谱-串联质谱法测定环境水中7种新烟碱类农药
Determination of 7 Neonicotinoid Pesticides in Environmental Water by Dispersion Liquid-Liquid Microextraction Combined with UPLC-MS/MS
摘要
Abstract
The dispersion liquid-liquid microextraction assisted by pasteurized dropper(PTD-DLLME)combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous determination of 7 neonicotinoid pesti-cides in environmental water.In the experiment,a pasteurized dropper was used as the extractor,acetonitrile with low density and low toxicity was used as the extractant,and acetone was used as the dispersant for the first time.The separation was performed on a BEH C18 column(2.1 mm×50 mm,1.7 µm)by gradient elution,with 0.01%formic acid aqueous solution(containing 2 mmol/L ammo-nium formate)and 0.01%formic acid acetonitrile solution(containing 2 mmol/L ammonium formate)as the mobile phases.After optimization of the gradient elution procedures and mass spectrometric conditions,chromatographic separation and feature recognition of the 7 neonicotinoid pesticides were obtained.Moreover,the optimal extraction conditions were determined as follows:sampling volume was 10 mL,extraction salt was 1 g NaCl and 4 g MgSO4,extractant was acetonitrile(800 µL),and dispersant was acetone(400 µL),which was confirmed by the best extraction efficiency in the sam-ple pretreatment.Analytes were scanned in positive ion mode by electrospray ionization source(ESI)under multiple reaction monitoring(MRM)mode,qualitated by retention time and characteristic ion,and quantitated by external standard method.Under the optimal conditions,the linear relationship of target compounds were good in the range of 0.05-100 µg/L with the correlation coefficients(r2)not less than 0.996.The limits of detection(LOD)were in the range of 0.02-0.1 µg/L,while the limits of quantitation(LOQ)were in the range of 0.05-0.2 µg/L,and the enrichment ratio was 10 times.At the spiked levels of 1,2 and 10 times LOQ,the recoveries of the analytes ranged from 75.3%to116%,and the relative standard deviations of intraday(Intra-RSDs,n=6)were 2.7%-8.2%and that of interday(Inter-RSDs,n=3)were 3.1%-10%.The matrix effects of the 7 neonicotinoid pesti-cides ranged from-0.18%to 6.66%.The established method was applied to 20 batches of environ-mental water samples,in which imidacloprid and thiacloprid were detected in one river water sam-ple,but their concentrations were below LOQ.This study indicated that PTD-DLLME combined with UPLC-MS/MS is an effective analytical method to detect 7 neonicotinoid pesticides in environ-mental water.The method is easy to operate,has a good enrichment effect,and offers stable recov-ery,environment friendly,and low cost,providing a new solution for the detection of neonicotinoid pesticides in environmental water samples.关键词
环境水/巴氏滴管/分散液液微萃取/超高效液相色谱-串联质谱/新烟碱类农药Key words
environmental water/pasteurized dropper/DLLME/UPLC-MS/MS/neonicotinoid pesticides分类
化学化工引用本文复制引用
侯新茹,仝凯旋,陈辉,张虹艳,常巧英,李相阳,李玲,薛晓晶..分散液液微萃取/超高效液相色谱-串联质谱法测定环境水中7种新烟碱类农药[J].分析测试学报,2024,43(5):738-745,8.基金项目
国家重点研发计划(2022YFC3700901) （2022YFC3700901）
国家乳业技术创新中心支持项目(2023-KFKT-28) （2023-KFKT-28）
