高效液相色谱-串联质谱法测定中草药中多种 新烟碱类农药的残留量

目的建立液相色谱-串联质谱分析法同时测定中草药夏枯草、野菊花、金银花、苏银花中噻虫嗪、氯噻啉、吡虫啉、啶虫脒、噻虫胺、噻虫啉6种新烟碱类农药残留量。方法样品中的6种新烟碱类杀虫剂经乙腈提取,QuEChERS方法净化后,液相色谱-串联质谱法分离和测定,外标法定量。结果方法检出限为0.1～4.8μg/kg,在方法的检测限与200 ng/mL测定范围内有良好的线性关系(r0.9990),在所添加5个水平浓度下,方法的回收率在70.4%～108.3%,相对标准偏差在1.0%～8.8%。结论该方法准确、简单、快速,适用于中草药中多种新烟碱类农药的同时检测。

Determination of residues of various neonicotinoid insecticides in Chinese herbal medicine by high performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for simultaneous determination of 6 neonicotinoid insecticides residues (thiamethoxam, imidaclothiz, imidacloprid, acetamiprid, clothianidin and thiacloprid) in Chinese herbal medicine of selfheal, wild chrysanthemum, honeysuckle, and honeysuckle bud by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Totally 6 neonicotinoid insecticides in the sample were extracted by acetonitrile, purified by QuEChERS method, separated and determined by liquid chromatography-tandem mass spectrometry, and quantified by external standard method. Results The limits of detection of the method were 0.1-4.8 g/kg, and there were good linear relationships between the limits of detection of the method and the determination range of 200 ng/mL (r>0.9990). The recoveries of the method were 70.4%-108.3% and the relative standard deviations were 1.0%-8.8% at the addition of 5 levels of concentration. Conclusions The method is accurate, simple and rapid, which is suitable for simultaneous detection of several neonicotinoid pesticides in Chinese herbal medicine.