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QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留
引用本文:杨路平, 邵立君, 王国玲, 王锡宁, 任晓菲, 刘拥军. QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留[J]. 食品工业科技, 2019, 40(14): 247-253. DOI: 10.13386/j.issn1002-0306.2019.14.040
作者姓名:杨路平  邵立君  王国玲  王锡宁  任晓菲  刘拥军
作者单位: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
基金项目: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5.0 g用乙腈-水(4:1)15 mL超声提取,经N-丙基乙二胺(PSA)30.0 mg和无水硫酸镁15.0 mg分散固相萃取吸附剂净化。使用HSS T3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0.5~200 μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3)0.03~0.3 μg/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。

关 键 词:QuEChERS  液相色谱-串联质谱法  食用菌  农药残留
收稿时间:2018-07-11

Determination of Thirteen Pesticides in Edible Mushrooms by QuEChERS with UPLC MS/MS
YANG Lu-ping, SHAO Li-jun, WANG Guo-ling, WANG Xi-ning, REN Xiao-fei, LIU Yong-jun. Determination of Thirteen Pesticides in Edible Mushrooms by QuEChERS with UPLC MS/MS[J]. Science and Technology of Food Industry, 2019, 40(14): 247-253. DOI: 10.13386/j.issn1002-0306.2019.14.040
Authors:YANG Lu-ping  SHAO Li-jun  WANG Guo-ling  WANG Xi-ning  REN Xiao-fei  LIU Yong-jun
Affiliation:1. Preventive medicine Research Institute of Shandong University, Jinan 250012, China;2. Shandong Center for Disease Control and Prevention, Jinan 250012, China;3. Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan 250062, China
Abstract: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.
Keywords:QuEChERS  UPLC MS /MS  edible mushrooms  pesticides residue
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