摘要
目的建立应用分散固相萃取-液相色谱质谱/质谱法同时测定茶叶中吡虫啉、啶虫脒、茚虫威和氯虫苯甲酰胺农药残留的方法。方法样品经乙腈,无水硫酸镁提取,离心后取有机相以N-丙基乙二胺(PSA)和无水硫酸镁作为分散固相萃取试剂去除杂质,浓缩后以乙腈定容,液相色谱-质谱/质谱检测。对超声提取的温度和时间以及PSA用量进行了优化,获得了最佳的超声萃取条件,优化了质谱条件。结果 4种杀虫剂在0μg/L～200μg/L浓度内线性关系良好(r值为0.996 9～0.999 9),检出限为0.000 3 mg/kg,低、中、高3个加标水平下回收率分别为72.1%～82.6%、74.5%～85.2%、70.3%～83.1%,相对标准偏差(RSD)为0.6%～4.5%。结论该方法操作简便,试剂消耗量少,回收率稳定,结果准确,适合同时检测茶叶中吡虫啉、啶虫脒、茚虫威和氯虫苯甲酰胺农药残留。
Objective To establish a method for the simultaneous determination of imidacloprid,acetamiprid,indoxacarb and chlorantraniliprole pesticide residues in tea by dispersive solid-phase extraction(DSPE)and liquid chromatography tandem mass spectrometry(LC-MS/MS).Methods The samples were extracted with acetonitril and anhydrous magnesium sulfate.After centrifugation,the organic phase was purified with primary secondary amine(PSA)and anhydrous magnesium sulfate as the dispersive solid phase extraction reagent.After concentration ,acetone was quantified by LC-MS/MS.The amounts of PSA ,the temperature and the time of ultrasonic extraction were optimized to obtain the best ultrasonic extraction conditions.Furthermore,the conditions of mass spectrometry were optimized.Results The linear relationship for four kinds of pesticides was good within 0 μg/L-200 μg/L,and the correlation coefficient(r)was within 0.9969-0.9999.The detection limit was 0.0003 mg/kg,the recoveries of three spiking levels were within 72.1%-82.6%,74.5%-85.2% and 70.3%-83.1 % respectively,and the relative standard deviation(RSD)was within 0.6%-4.5%.Conclusion The method is easy to operate,with less reagent consumption,stable recoveries,accurate and reliable results,which is suitable for simultaneous determination of imidacloprid,acetamiprid,indoxacarb and chlorantraniliprole pesticide residues in tea.
作者
黄季维
樊文明
梅玉琴
廖青
李谦
刘天洁
HUANG Ji-wei;FAN Wen-ming;MEI Yu-qin;LIAO Qing;LI Qian;LIU Tian-jie(Zigong Center for Disease Control and Prevention,Zigong,Sichuan 643000,China)
出处
《中国卫生检验杂志》
CAS
2019年第7期778-781,共4页
Chinese Journal of Health Laboratory Technology
关键词
分散固相萃取
液相色谱-质谱/质谱
茶叶
农药残留
Dispersive solid phase extraction
Liquid chromatography tandem-mass spectrometry
Tea
Pesticide residue
