LC-MS技术快速分析稻米中毒死蜱和丁硫克百威及其代谢产物的残留量.pdf

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LG-MS技术快速分析稻米中毒死蜱和丁硫克
百威及其代谢产物的残留量
杨欢,马有宁,秦关玲,柴炎炎,何巧,张涵彤,牟仁样
中国水将研究所,农化部将米及制品质宝监督检验测试中心,农业部将米产品质宝安全风险评估实验室,
浙江杭州310006
摘要:建立了高效汶相色谱-质谐联( liquid chromatography- -tandem mass spcctromctry,IC-MSMS)快速测定稻米
中2种杀虫剂(毒死蜱和丁硫克百威)及有毒代谢产物(克百威、3-羟基克百威和3、5,6-TCP)多残留的方法。样品经
酸化的乙提取,PSA和C两和分散?相萃取剂净化,并以甲崞-含0.1%甲酸的5 mio/L甲酸铵水溶液为流动和梯
度洗脱,采川 Eclipse XI)B-C18柱色譜杜分离,正负离子模式切换扫描,多反应监测(MRM)定性分析口标化合物
实验通过比较提取溶剂中小同浓度的酸对样品提取效率的影响,进步优化 QUECHERS方法,提高了方法的灵敏
度。5种分析物在0.2~10000gL浓度范内线性良好,相关系数R0.998,方法检出限为0.3~1.7ugkg:定量限
为1.0-5.0gkg。各种分析物在空自基质中的3个添加水半(1、10、100和5、25、125gkg)下?收率为72.0%
99.6%,柑?标准偏差(RSD.m=6)沱围为0.6%~12%。实验结果表明该方法快速、向效,适用于稲米样品中毒死坤
和∫硫克白成及代谢物的快速测定。
关键词:液相色谱-联质谱(IC-MSMS); QUECHERS:农药;代谢物;稻米
Rapid Analysis of Chlorpyrifos and Carbosulfan and Toxic
Metabolites residual in Rice by LC-MS
YANG Huan, MA Youning, QIN Meiling, CHAI Shuangshuang, HH Qiao,/HAN( Hantong, MOU! Renxiang
Rice Product Quality Inspection and Supervision Center, Mistry of Agriculture, Laboratory of Quality and Safety Risk
Assessmenl for Ricc, Ministry o[ Agriculture, China National Rice Research Instilute, I hou 310006, China)
bstract: A method was developed for the rapid determination of two pesticides(chlorpyrifos and carbosulfan)and toxic
metabolites (carbofuran, 3-hydroxycarbofuran and 3, 5. 6-TCP) residues in polished rice by high performance liquid
chromatography-landcm mass spcctromctry (. C-MS MS). The five analytes were extracted from samples by acidified
acetonitrile and purified by two solid phase extraction agents of Cu& and PSA. The five compounds were separated on a
Eclipse XDB-C18 column by the gradient elution using methamol-0.1%(w/)formic acid and 5mmoll formic acetate
aqucous solution as mobile phases, delected by MS/MS with positive and negative ion mode scanning and finally quantified
in multiple reaction monitoring(MRM)mode. In order to optimize the QUECHERS method and improve the sensitivity of the
method, the exiraction elliciency of differenl concentrations of formic acid in acetonitrile was compared. The correlalion
收稿口期:2017-09-05
基金项目:国家农产品质星安全风险评估项目(GIP2016001001)、中央级公慌性科研院所基本科研业务费专项资金
项H(2014RG006)
作者简介:杨欢(1991-),女,顽士,研究方向为农约风险评佔研究,E-mai:15267498845(a163.com
*通计作者:弁仁(1976-),男,副研究员,本科,研究方向为农产品质量安全风险评估技术研究, Email
mrcnxiang(@163.com