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气相色谱 - 三重四极杆质谱法在痕量水平鸡蛋中农药和多氯联苯定量确证中的应用

Application of gas chromatography-triple quadrupole mass spectrometry in the quantification-confirmation of pesticides and polychlorinated biphenyls in eggs at trace levels.

作者信息

Bolaños P Plaza, Frenich A Garrido, Vidal J L Martínez

机构信息

Research group Analytical Chemistry of Contaminants, Department of Analytical Chemistry, University of Almería, 04120 Almería, Spain.

出版信息

J Chromatogr A. 2007 Oct 5;1167(1):9-17. doi: 10.1016/j.chroma.2007.08.019. Epub 2007 Aug 12.

Abstract

A new multiresidue method has been developed and validated for the simultaneous analysis of 57 compounds, including organochlorine and organophosphorus pesticide residues (OCPs and OPPs) and polychlorinated biphenyls (PCBs), in eggs at trace levels by gas chromatography coupled to triple quadrupole mass spectrometry (GC-QqQ-MS/MS). Egg samples were extracted by a simple and fast matrix solid phase dispersion (MSPD) procedure using C18 as sorbent, and ethyl acetate and acetonitrile saturated in n-hexane (85:15, v/v) as elution solvent with a simultaneous clean up with Florisil in-line. The QqQ analyzer acquired data in selected reaction monitoring (SRM) mode, permitting both quantification and confirmation in a single injection with a running time reduced up to 17.70 min. Recovery was in the range of 70-110% and 70-106% at 15 and 50 microg/kg, respectively. Precision values expressed as relative standard deviation (RSD) were lower than 20%. Linearity in the range of 10-150 microg/kg provided determination coefficients (R(2)) higher than 0.98 for all compounds. Limits of detection (LODs) for pesticides were < or =2.25 microg/kg and limits of quantification (LOQs) ranged from 0.02 to 7.78 microg/kg. LODs for PCBs were < or =0.41 microg/kg and LOQ were < or =0.71 microg/kg. The method was applied to real samples. Endosulfan sulphate and p,p'-DDE were found in two samples at concentrations below the first calibration level.

摘要

已开发并验证了一种新的多残留方法,用于通过气相色谱-三重四极杆质谱联用(GC-QqQ-MS/MS)同时分析鸡蛋中痕量水平的57种化合物,包括有机氯和有机磷农药残留(OCPs和OPPs)以及多氯联苯(PCBs)。鸡蛋样品采用简单快速的基质固相分散(MSPD)程序进行提取,使用C18作为吸附剂,用乙酸乙酯和正己烷饱和的乙腈(85:15,v/v)作为洗脱溶剂,并同时在线用弗罗里硅土进行净化。QqQ分析仪在选择反应监测(SRM)模式下采集数据,一次进样即可实现定量和确证,运行时间缩短至17.70分钟。在15和50微克/千克时,回收率分别在70-110%和70-106%范围内。以相对标准偏差(RSD)表示的精密度值低于20%。在10-150微克/千克范围内的线性关系使得所有化合物的测定系数(R(2))高于0.98。农药的检测限(LODs)≤2.25微克/千克,定量限(LOQs)范围为0.02至7.78微克/千克。PCBs的LODs≤0.41微克/千克,LOQ≤0.71微克/千克。该方法应用于实际样品。在两个样品中发现了低于第一个校准水平浓度的硫丹硫酸酯和p,p'-滴滴伊。

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