增强型脂质去除固相萃取净化-超高效液相色谱-串联质谱法测定贝类中42种除草剂残留

Determination of 42 Herbicides Residues in Shellfish Using Captiva EMR-Lipid Clean-up in Combination with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

为建立一种基于增强型脂质去除(Captiva EMR-Lipid)固相萃取技术的贝类中42种三嗪类、酰胺类及磺酰脲类除草剂残留的超高效液相色谱-串联质谱(UPLC-MS/MS)同时快速分析方法,对贝类样品的提取与净化方式、色谱与质谱分析条件等进行优化。以乙腈为提取溶剂,以增强型脂质去除固相萃取净化,目标化合物经Shim-pack GIST C18-AQ(100mm×2.1 mm,1.9μm)色谱柱分离、梯度洗脱。使用电喷雾正离子模式,以多反应监测(MRM)模式采集。结果表明,在0.2~20μg/L线性范围,42种目标化合物的线性相关系数(R2)均大于0.992,方法检出限及定量限分别为0.2~0.4μg/kg和0.5~1.0μg/kg,平均回收率为61.0%~110.3%,相对标准偏差为0.1%~17.4%。利用该方法对23批次实际样品进行分析测定,共检出5种除草剂。该方法简便高效,具有较好的准确度和灵敏度,适用于贝类中42种除草剂多残留测定。

Based on enhanced matrix removal lipid column(Captiva EMR-Lipid)purified,a method was developed for determination of 42 kinds of triazine,amide and sulfonylurea herbicides residues in shellfish by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).After optimizing the pretreatment and chromatographic conditions,acetonitrile,Captiva EMR-Lipid column were used as the extraction solvents and purification agents,respectively.The separation of 42 analytes was performed on a Shim-pack GIST C18-AQ column(100 mm×2.1 mm,1.9μm)with gradient elution.The MS/MS detection was performed with electrospray ionization in positive ion mode and multiple reaction monitoring mode.The 42 analytes showed great linear relationships in the range of 0.2-20μg/L with correlation coefficients(R~2)all above 0.992.The limits of detection(LODs)were 0.2-0.4μg/kg and the limits of quantitation(LOQs)were 0.5-1.0μg/kg.The average recoveries of analytes varied from 61.0%to 110.3%,and the relative standard deviations(RSDs)were between 0.1%and 17.4%.Using the established determination method,23 shellfish samples were detected,and 5 kinds of herbicides residues were detected.The method was simple,rapid,high accurate and sensitive,which was suitable for the simultaneous determination of 42 kinds of herbicides residues in shellfish.