QuECHERS-液相色谱-串联质谱法测定不同产地人参中147种农药残留  

Determination of 147 pesticide residues in Panax ginseng from different producing areas by QuECHERS-liquid chromatography-tandem mass spectrometry

作　　者：王嘉琦 金书含 高海云 孔凡字 辛国松[1] 于淼[1] 綦峥[1] WANG Jia-qi;JIN Shu-han;GAO Hai-yun;KONG Fan-zi;XIN Guo-song;YU Miao;QI Zheng(Engineering Research Center for Medicine,Ministry of Education,Harbin University of Commerce,Harbin 150076,China)

机构地区：[1]哈尔滨商业大学国家教育部药物工程技术研究中心,黑龙江省哈尔滨150076

出　　处：《中草药》2023年第14期4662-4671,共10页Chinese Traditional and Herbal Drugs

基　　金：哈尔滨商业大学2022年研究生创新科研基金项目(YJSCX2022-754HSD);中央支持地方高校改革发展基金优秀青年人才项目(2020YQ12);黑龙江省自然科学基金优秀青年基金项目(YQ2022H002);黑龙江省卫生健康委员会科技计划(2020-196)。

摘　　要：目的 建立QuEChERs结合液相色谱-串联质谱同时测定不同产地人参Panax ginseng中147种农药残留的分析方法。方法 人参样品经0.1%冰醋酸乙腈提取,QuEChERs法净化,采用F5色谱柱(50 mm×30 mm,2.6μm),流动相为0.5%氨水-0.1%甲酸水溶液(A)-甲醇(B);进样口温度为250℃,进样量为10μL,体积流量0.5 mL/min,电离方式ESI+;毛细管电压5.5 kV;源温度500℃;气帘气压力207 kP a:雾化器压力414 kP a;碰撞气62 kP a,多反应监测模式。结果 147种农药的线性关系良好,相关系数均不低于0.995,3个添加水平(1.0、5.0、20.0ng/kg)下,81.2%的农药残留的回收率范围在60%~140%,相对标准偏差均小于14.02%。结论 该方法净化方式简单、提取充分、回收率较高,适用于人参中农药残留的筛查测定,为人参中农药残留量的快速筛查和质量控制提供技术支撑。Objective To establish an analytical method for the simultaneous determination of 147 kinds of pesticide residues in Panax ginseng by QuEChERs combined with liquid chromatography-tandem mass spectrometry.Methods The sample was extracted by 0.1% acetic acid glacial-acetonitrile and purified by QuEChERs method on F5 column(50 mm × 30 mm,2.6 μm),mobile phase:0.5% ammonium hydroxide-0.1% formic acid water solution(A)-methanol;Inlet temperature:250 ℃,injection volume:10 μL,flow rate:0.5 mL/min,ionization method:ESI+;capillary voltage:5.5 kV;source temperature:500 ℃;gas curtain air pressure:207 kP a:nebulizer pressure:414 kP a;collision gas:62 kP a,multi-reaction monitoring mode.Results The mass concentration of 147 pesticides had good linear relationship with correlation coefficients higher than 0.995.The average recoveries of 81.2% pesticides in ginseng ranged from 60% to 140% in three spiked levels(1.0,5.0,20.0 ng/kg),and the relative standard deviations were all less than 14.02%.Conclusion This method is simple in purification,sufficient in extraction and high in recovery rate.The result has certain reference value for cultivation and circulation supervision of ginseng,which can provide technical support for rapid screening and quality control of pesticides in ginseng.

关 键 词：人参 农药残留 QuEChERs法 液相色谱-串联质谱法 质量控制 

分 类 号：R286.2[医药卫生—中药学]