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高效液相色谱-串联质谱法测定婴幼儿谷物食品中11种苯氧羧酸类除草剂
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王可,曹倩玉,赵灵芝,陈龙星,张梦妍 石家庄市疾病预防控制中心理化检验所 
基金项目:“十三五”国家重点研发计划项目(2016YFD0300708)
中文摘要:建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时检测婴幼儿谷物食品中11种苯氧羧酸类除草剂的分析方法。试样采用含2%甲酸的乙腈溶液提取,以N-丙基乙二胺(PSA)和无水硫酸镁(MgSO4)净化后,经ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×50 mm,1.8 μm)分离,采用电喷雾离子源 (ESI)负离子,多反应监测(MRM)模式进行检测,外标法定量。11种苯氧羧酸类除草剂在0.5~200 μg/L范围内线性关系良好,相关系数(r2)均大于0.999,在3个加标水平下的平均回收率为77.4%~99.9%,相对标准偏差(RSD,n=7)为1.5%~8.0%,方法的检出限(S/N=3)为0.1~2.4 μg/kg ,定量下限(S/N=10)为0.4~8.1 μg/kg。该方法操作简便、准确度高、灵敏度好,适用于婴幼儿谷物食品中11种苯氧羧酸类除草剂的快速同时检测。
中文关键词:高效液相色谱-串联质谱(HPLC-MS/MS)  苯氧羧酸类除草剂  QuEChERS  婴幼儿谷物食品
 
Determination of 11 Phenoxy Acid Herbicides in Infant Cereal Food by High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A method was developed for the simultaneous determination of 11 phenoxy acid herbicides in infant cereal food by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted with acetonitrile containing 2% formic acid,then purified with N propyl ethylenediamine(PSA) and anhydrous magnesium sulfate(MgSO4).The target compounds were separated on a ZORBAX Eclipse XDB-C18 column(4.6 mm×50 mm,1.8 μm),and detected by HPLC-MS/MS with electrospray ionization(ESI) in negative ion mode under multiple reaction monitoring(MRM) mode,and quantified by the external standard method.The calibration curves for 11 phenoxy acid herbicides were linear in the range of 0.5-200 μg/L with their correlation coefficients(r2) larger than 0999.The average recoveries at 3 spiked levels were in the range of 77.4%-999%,with relative standard deviations(RSDs,n=7) of 1.5%-8.0%.The limits of detection(S/N=3) and quantitation(S/N=10) of the method were 0.1-2.4 μg/kg and 0.4-8.1 μg/kg,respectively.Owing to the advantages of simple operation,high accuracy and sensitivity,this method is suitable for the rapid and simultaneous detection of 11 phenoxy acid herbicides in infant cereal food.
Key Words:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  phenoxy acid herbicides  QuEChERS  infant cereal food
引用本文:王可,曹倩玉,赵灵芝,陈龙星,张梦妍.高效液相色谱-串联质谱法测定婴幼儿谷物食品中11种苯氧羧酸类除草剂[J].分析测试学报,2018,37(11):1349-1353.
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