加速溶剂萃取-固相萃取净化-气相色谱-串联质谱法检测茶叶中9种拟除虫菊酯类农药残留  

Determination of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry combined with accelerated solvent extraction and solid phase extraction

作　　者：黄微 李娜 徐瑞晗 李婷 李崇勇 HUANG Wei;LI Na;XU Ruihan;LI Ting;LI Chongyong(Hanzhong Control and Testing Center for Food and Drug,Hanzhong 723000,China;Hanzhong Animal Hygienie Supervision Institute,Hanzhong 723000,China)

机构地区：[1]汉中市食品药品检验检测中心,陕西汉中723000 [2]汉中市动物卫生监督所,陕西汉中723000

出　　处：《色谱》2018年第12期1303-1310,共8页Chinese Journal of Chromatography

摘　　要：建立了加速溶剂萃取(ASE)-固相萃取净化(SPE)-气相色谱-串联质谱(GC-MS/MS)同时测定茶叶中9种拟除虫菊酯类农药残留的方法。ASE萃取溶剂为丙酮-正己烷(1∶1,v/v),萃取温度为100℃,萃取压力为10 MPa,加热时间为3 min,静态萃取时间为5 min,循环1次,冲洗体积为40%萃取池体积,氮气吹扫100 s。萃取结束后用Cleanert TPT固相萃取柱净化,净化液浓缩定容后,采用GC-MS/MS测定,外标法定量。9种拟除虫菊酯类农药在2～1 000μg/L范围内呈现良好的线性关系,相关系数(r2)均大于0. 99,方法检出限为0. 2～4. 5μg/kg,定量限为0. 8～15. 0μg/kg。在绿茶、红茶空白基质中做加标回收试验,添加水平为0. 02、0. 1、0. 4 mg/kg以及定量限水平,得到的平均回收率为69. 87%～110. 0%,相对标准偏差(RSD)为0. 7%～11. 2%。该方法背景干扰低、灵敏度高、重现性好、回收率稳定,适用于茶叶中拟除虫菊酯类农药残留量的检测。A method has been developed for the simultaneous detection of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry(GC-MS/MS)combined with accelerated solvent extraction(ASE)and solid-phase extraction(SPE).The pesticide residues in tea were extracted using acetone/n-hexane(1∶1,v/v)for 5 min at 100℃before preheating the extraction pool for 3 min,under extractive pressure of 10 MPa for one cycle.After extraction,the extraction pool was washed with acetone/n-hexane(1∶1,v/v)having volume of 40%of the pool volume,followed by purging for 100 s with nitrogen.The extract was purified by a Cleanert TPT solid-phase extraction column.After purification,the target compounds were detected by GC-MS/MS and quantified by the external standard method.Under the optimized conditions,good linearities were obtained for the nine pyrethroid pesticides in the range of 2-1 000μg/L,with correlation coefficients exceeding 0.99.The limits of detection(LODs)were 0.2-4.5μg/kg and the limits of quantitation(LOQs)were 0.8-15.0μg/kg.At four spiked levels(0.02,0.1,0.4 mg/kg,and the LOQ level)in green tea and black tea,the recoveries of all the pesticides were between 69.87%and 110.0%,with relative standard deviations(RSDs)varying from 0.7%to 11.2%.This method effectively reduces the matrix interference and shows high sensitivity,good reproducibility,and stable recovery,and can thus be used for the detection of pyrethroid pesticide residues in tea.

关 键 词：气相色谱-串联质谱 加速溶剂萃取 拟除虫菊酯类农药 茶叶 

分 类 号：O658[理学—分析化学]