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气相色谱-三重四极杆质谱联用仪分析草莓中151种农药残留的多残留方法的建立与验证

Development and validation of a multiresidue method for the analysis of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer.

作者信息

Bolaños Patricia Plaza, Moreno José Luis Fernández, Shtereva Deyana D, Frenich Antonia Garrido, Vidal José Luis Martínez

机构信息

Department of Analytical Chemistry, University of Almería, 04071 Almería, Spain.

出版信息

Rapid Commun Mass Spectrom. 2007;21(14):2282-94. doi: 10.1002/rcm.3091.

Abstract

A new method was developed and validated for the simultaneous determination of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer (GC/QqQ-MS/MS), mainly using the selected reaction monitoring (SRM) mode. The list of target compounds included various classes of pesticides such as organochlorine (OCPs), organophosphorus (OPPs), carbamates, pyrethroids, triazoles and dicarboximides. A single extraction of 10 g of sample with acetonitrile followed by liquid-liquid partition formed by the addition of 4 g of MgSO4 and 1 g of NaCl was applied in sample preparation. Cleanup of the extracts was carried out by applying dispersive solid-phase extraction (D-SPE) with primary secondary amine (PSA). The analysis time was 21 min. The method was subjected to a thorough validation procedure. The recovery data were obtained by spiking blank samples at two concentration levels (11.5 and 50 microg/kg), yielding recoveries in the range 70-110%. Precision values expressed as relative standard deviation (RSD) were lower than 18% and 22% for the intraday and interday precision, respectively. Linearity was studied in the range 10-200 microg/kg and determination coefficients (R(2)) were higher than 0.98% for all compounds. Limits of detection (LODs) and limits of quantification (LOQs) were established as 4 and 10 microg/kg, respectively. The overall uncertainty of the method was estimated at two different concentrations (11.5 and 50 microg/kg), being lower than 25% in both cases. According to the validation data and performance characteristics as well as the high sample throughput and low cost, the proposed method is suitable for routine application.

摘要

开发并验证了一种新方法,用于通过气相色谱-三重四极杆质谱仪(GC/QqQ-MS/MS)同时测定草莓中的151种农药残留,主要采用选择反应监测(SRM)模式。目标化合物列表包括各类农药,如有机氯农药(OCPs)、有机磷农药(OPPs)、氨基甲酸酯类、拟除虫菊酯类、三唑类和二羧酰亚胺类。样品制备采用10 g样品用乙腈单次萃取,然后加入4 g硫酸镁和1 g氯化钠进行液液分配。提取物的净化通过用伯仲胺(PSA)进行分散固相萃取(D-SPE)来实现。分析时间为21分钟。该方法经过了全面的验证程序。通过在两个浓度水平(11.5和50 μg/kg)对空白样品进行加标获得回收率数据,回收率范围为70-110%。日内和日间精密度分别以相对标准偏差(RSD)表示,精密度值分别低于18%和22%。在10-200 μg/kg范围内研究线性,所有化合物的测定系数(R²)均高于0.98%。检测限(LOD)和定量限(LOQ)分别确定为4和10 μg/kg。在两个不同浓度(11.5和50 μg/kg)下估计了该方法的总体不确定度,两种情况下均低于25%。根据验证数据和性能特征以及高样品通量和低成本,所提出的方法适用于常规应用。

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