采用UPLC快速检测中药材中七种新烟碱类杀虫剂的方法探索

The UPLC method of rapid detection of seven neonicotinoid insecticides in Chinese medicinal materials

目的:本研究旨在建立一种能检测人参、三七、西洋参三种中药材中七种新烟碱类杀虫剂的超高液相色谱分析方法。方法:本研究以ACQUITY HSS T3(2.1 mm×50 mm,1.8μm)色谱柱为固定相;以0.3%甲酸-水为水相(A),含5 mmol·L^(-1)甲酸铵乙腈(B)为有机相;检测波长为254 nm,通过优化前处理方法以及检测条件,建立了超高效液相色谱分析方法。该方法能够检测三七、西洋参、人参三种药食同源的中药材中的噻虫嗪、啶虫脒、氯噻啉、啶虫脒、吡虫啉、氟吡呋喃酮、噻虫啉等7种新烟碱类杀虫剂残留。结果:本研究成功建立一种能检测中药材中多种新烟碱类杀虫剂的超高液相色谱方法。液相梯度洗脱条件:0~1 min 95%A;5%B,1~13 min 95%A→55%A,13~14 min 55%A→95%A,14~15 min 95%A;5%B。在基质检测中,人参检测灵敏度最高,检出限在18.33~79.34μg·kg^(-1)之间,定量限在61.10~264μg·kg^(-1)之间。三七检测灵敏度最低,检出限在20.33~143.13μg·kg^(-1)之间,定量限在67.73~477.11μg·kg^(-1)之间。西洋参检出限在24.68~108.38μg·kg^(-1)之间,定量限在82.28~361.28μg·kg^(-1)之间。检测的10批三七、2批人参、7批西洋参中均没有相关检出。结论:本研究建立的超高效液相色谱方法适用于三七、西洋参、人参三种中药材中7种新烟碱类杀虫剂快速检测,供同行参考。

Objective:The aim of this study was to establish an ultra-high liquid chromatography method for the detection of seven neonicotinoid insecticides in Renshen,Sanqi and Xiyangshen.Method:In this study,ACQUITY HSS T3(2.1 mm×50 mm,1.8μm)column was used as stationary phase.0.3%formic acid-water was used as the aqueous phase(A),containing 5 mmol·L^(-1)ammonium formate acetonitrile(B)as organic phase.A detection wavelength was set at 254 nm.An ultra-high performance liquid chromatography method was established by optimizing the pretreatment method and detection conditions.The method can detect the residues of 7 kinds of neonicotinoid insecticides,such as thiamethoxam,chlorthiazidine,chlorthiazoline,imidacloprid,fluopyrifuranone and thiacloprid in three kinds of Chinese medicinal materials of homology of medicine and food Sanqi,Xiyangshen and Renshen.Result:In this study,an ultra-high liquid chromatography method for the detection of neonicotinoid insecticides in Chinese medicinal materials was successfully established.Gradient elution conditions were as follows:0~1 min 95%A,5%B,1~13 min 95%A→55%A,13~14 min 55%A→95%A,14~15 min 95%A,5%B.The detection limit and sensitivity were highest for Renshen,with detection limits ranging from 18.33 to 79.34μg·kg^(-1)and limits of quantification ranging from 61.10 to 264μg·kg^(-1).The detection limit and sensitivity were lowest for Sanqi,with detection limits ranging from 20.33 to 143.13μg·kg^(-1)and limits of quantification ranging from 67.73 to 477.11μg·kg^(-1).The limits of detection for Xiyangshen was 24.68~108.38μg·kg^(-1),and the limits of quantification were 82.28~361.28μg·kg^(-1).No neonicotinoid insecticides were detected in 10 batches of Sanqi,2 batches of Renshen and 7 batches of Xiyangshen.Conclusion:The ultra-high performance liquid chromatography method developed in this study can be applied to the rapid detection of seven neonicotinoid insecticides for reference in three kinds of Chinese medicinal materials Sanqi,Xiyangshen and Renshen.