超高效液相色谱-串联质谱法快速筛查茶叶中的多种农药残留  

Rapid screening of multi-residue pesticides in tea by UPLC-MS / MS

作　　者：韩璐[1,2] 陈达炜[2] 吕冰[2] 苗虹[1,2] 

机构地区：[1]中国疾病预防控制中心营养与健康所,北京100050 [2]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京100021

出　　处：《中国食品卫生杂志》2015年第4期386-393,共8页Chinese Journal of Food Hygiene

基　　金：国家国际科技合作专项(2011DFA31770)

摘　　要：目的采用超高效液相色谱-串联质谱技术(UPLC-MS/MS)和改进的Qu ECh ERS样品前处理技术,建立茶叶中多种农药残留的快速筛查检测方法。方法样品采用乙腈提取,提取液经N-丙基乙二胺(PSA)、石墨化炭黑(GCB)及茶叶农残检测专用吸附剂(TPT)混合进行分散固相萃取净化(d-SPE)。以BEH C18色谱柱(2.1 mm×100 mm,1.7μm)进行色谱分离,以电喷雾电离串联质谱多反应监测模式(MRM)进行监测。结果以欧盟农药残留参比实验室组织的茶叶中175种农药残留的国际比对考核的茶叶样品进行定性筛查和定量测定,以液相色谱质谱技术从考核茶叶样品中共定性筛查出多菌灵、吡虫清、噻嗪酮等10种农药残留。针对这10种农药进行了定量检测方法的建立和方法验证,10种农药在0.1~20μg/L的浓度范围内呈良好线性,相关系数r>0.999,各农药的定量限为0.5~2.0μg/kg,茶叶样品基质的加标回收率在75.7%~105.8%之间,相对标准偏差在2.3%~18.4%之间。定量测得考核的茶叶样品中10种农药的含量在0.021~0.373 mg/kg之间。结论本方法简单、准确、灵敏度高,适用于农产品中农药多残留的快速筛查。Objective To establish a rapid screening and confirmation method for pesticide residues in tea using UPLC- MS/MS for instrument method and QuEChERS for sample preparation. Methods The pesticide residues were extracted from tea samples with acetonitrile, and purified by dispersion solid phase extraction （d-SPE） using N-propyl ethlene diamine （PSA）, graphitized carbon black （GCB） and triple phase of tea （TPT）. The pesticide analytes were then separated on a reversed phase column using a gradient elution program. The ion fragment were obtained using ultra high performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode and quantified by the external standard method. ResuLts In checking tea sample, 10 pesticide were screened qualitatively and carried on the quantitative analysis. The method showed a good linearity （r 〉 0. 999） in the ranges of O. 1-20μg/L for lO pesticide with average recovery rates of 75.7%-105.8% and the relative standard deviation （RSD） of 2.3%-18.4%. The limits of quantification （LOQs） for 10 pesticide were between 0. 5 and 2 p^g/kg. Conclusion The method was simple, sensitive and accurate, and was suitable for confirmation multi-residue pesticides in agricultural products.

关 键 词：超高效液相色谱-串联质谱 QUECHERS 农药残留 茶叶 食品污染物 风险监测 

分 类 号：R155.5[医药卫生—营养与食品卫生学] F767.2[医药卫生—公共卫生与预防医学]