UPLC-MS/MS测定鲜切康乃馨和柃木中农药多残留  

The Multi-Class Method for Determination of Pesticide Residues in Cut Live Plants by UPLC-MS/MS

作　　者：陈先锋[1] 湛嘉[1] 钟莺莺[1] 顾建锋[1] 俞雪钧[1] 彭锦峰[1] 冯睿[1] 王松青[1] 崔俊霞[1] 

机构地区：[1]宁波出入境检验检疫局,浙江宁波315012

出　　处：《检验检疫学刊》2012年第6期54-61,共8页Journal of Inspection and Quarantine

基　　金：国家质检总局课题(2011IK181);宁波市科技计划项目(2011C50082);宁波出入境检验检疫局课题(2008K03)

摘　　要：建立了一种同时分析鲜活植物—康乃馨和柃木中25种典型常用农药的通用、快速、简便的UPLC-MS/MS多残留分析方法。样品仅需通过乙腈提取和基质分散固相萃取(d-SPE)净化等简单处理。通过基质添加标准曲线定量,R2均高于0.994,线性良好。定量检测限为0.5 mg/kg。康乃馨平均添加回收率范围在84.7%-114.1%之间,RSD范围在2.2%-13.5%;柃木平均添加回收率范围在78.2%-115.8%之间,RSD范围在1.1%-15.7%。本方法具有简便、快速和通用的特点,能增加农药的种类覆盖范围和提高检测效率,省时省力,非常适合花卉、植物等产品农药残留检测。A generic,rapid and simple analytical method able to simultaneously identify 25 pesticide residues in cut live plants was developed.The method is based on extraction with acetonitrile,cleanup by D-SPE,and analysis by ultra performance liquid chromatography coupled with electrospray ionization and tandem mass spectrometry（UPLC–ESI–MS/MS） operating in positive multiple reaction mode（MRM）.Most of pigment and lipids in the extract were eliminated by the optimized sample preparation prior to analysis without any significant losses of the most of the analyses.For quantification,matrix-fortified calibration curves were performed to compensate for the matrix effect and loss in sample preparation.Good linearity was found for all target compounds with linear regression coefficients（R2） higher than 0.994.The method quantification limits（LOQs） was 0.5 mg/kg.Average recoveries for the spiked carnation were from 84.7 to 114.1% with associated RSD values from 2.2 to 13.5 %,and eurya japonica were from 78.2 to 115.8% with associated RSD values from 1.1 to 15.7 % under the selected conditions.The method has been validated for its extraction sensitivity,linearity,recoveries and precision.The results clearly demonstrate the feasibility of the simple,rapid and generic approach proposed,which improves the coverage of residues and efficiency.Application of the method in routine monitoring programs for cut live plants would imply a drastic reduction in both effort and time.

关 键 词：鲜切植物 超高效液相色谱-串联质谱 农药 多类别多残留 基质分散固相萃取 

分 类 号：O657.63[理学—分析化学]