QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留  

Determination of Thirteen Pesticides in Edible Mushrooms by QuEChERS with UPLC MS/MS

作　　者：杨路平 邵立君[1,2] 王国玲 王锡宁[1,2] 任晓菲 刘拥军[3] YANG Lu-ping;SHAO Li-jun;WANG Guo-ling;WANG Xi-ning;REN Xiao-fei;LIU Yong-jun(Preventive medicine Research Institute of Shandong University,Jinan 250012,China;Shandong Center for Disease Control and Prevention,Jinan 250012,China;Institute of Materia Medica,Shandong Academy of Medical Sciences,Jinan 250062,China)

机构地区：[1]山东大学预防医学研究院,山东济南250012 [2]山东省疾病预防控制中心,山东济南250012 [3]山东省医学科学院药物研究所,山东济南250062

出　　处：《食品工业科技》2019年第14期247-253,共7页Science and Technology of Food Industry

基　　金：山东省医药卫生科技发展计划(2015WS0273);山东省中医药科技发展计划(2017-182)

摘　　要：目的:建立并应用QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留。方法:样品5.0g用乙腈-水(4∶1)15mL超声提取,经N-丙基乙二胺(PSA)30.0mg和无水硫酸镁15.0mg分散固相萃取吸附剂净化。使用HSST3色谱柱,0.1%甲酸和乙腈为流动相梯度洗脱。质谱采用电喷雾正离子源和多反应监测模式。结果:13种农药的质量浓度在0.5~200μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3)0.03~0.3μg/kg。加标回收率84.3%~102%,相对标准偏差(n=6)2.8%~6.3%。结论:该方法可用于食用菌中13种农药残留的检测。Objective:Determination of thirteen pesticides in edible mushrooms by QuEChERS with UPLC MS /MS.Methods:5.0 g sample was extracted ultrasonically for 5 min with 15 mL of 4∶ 1 acetonitrile and water.The extract was purified by N- propyl ethylenediamine( PSA) 30.0 mg,anhydrous Magnesium sulfate 15.0 mg dispersive solid-phase extraction adsorbent.The purified solution was separated by UPLC using HSS T3 column,0.1% formic acid and acetonitrile as mobile phase in gradient elution. Positive ESI and MRM were adopted in MS analysis.Results:Linear relationships were found between the peak area and the mass concentration of 13 pesticides within 0.5~200 μg /L.With detection limits( S /N = 3) in the range of 0.03~0.3 μg /kg, recovery rates obtained by standard addition method ranged from 84.3% to 102% and RSDs( n = 6) were in the range of 2.8%~6.3%.Conclusion:The proposed method was successfully applied to the detection of 13 pesticides in mushrooms.

关 键 词：QUECHERS 液相色谱-串联质谱法 食用菌 农药残留 

分 类 号：TS207.5[轻工技术与工程—食品科学]