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

Determination of 11 Phenoxy Acid Herbicides in Infant Cereal Food by High Performance Liquid Chromatography-Tandem Mass Spectrometry

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. 8μm)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. 5～200μg/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. 4μg/kg,定量下限(S/N=10)为0. 4～8. 1μg/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。

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(MgSO 4).The target compounds were separated on a ZORBAX Eclipse XDB-C 18 column(4.6 mm×50 mm,1.8μm),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 0.5-200μg/L with their correlation coefficients(r 2)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 0.1-2.4μg/kg and 0.4-8.1μg/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.