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Multiresidue analysis of multiclass pesticides and polyaromatic hydrocarbons in fatty fish by gas chromatography tandem mass spectrometry and evaluation of matrix effect

机译:气相色谱串联质谱法对脂肪鱼中多种农药和多环芳烃的多残留分析及基质效应评估

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This paper reports a selective and sensitive method for multiresidue determination of 119 chemical residues including pesticides and polyaromatic hydrocarbons (PAH) in high fatty fish matrix. The novel sample preparation method involved extraction of the target analytes from homogenized fish meat (5 g) in acetonitrile (15 mL, 1% acetic acid) after three-phase partitioning with hexane (2 mL) and the remaining aqueous layer. An aliquot (1.5 mL) of the acetonitrile layer was aspirated and subjected to two-stage dispersive solid phase extraction (dSPE) cleanup and the residues were finally estimated by gas chromatography mass spectrometry with selected reaction monitoring (GC-MS/MS). The co-eluted matrix components were identified on the basis of their accurate mass by GC with quadrupole time of flight MS. Addition of hexane during extraction and optimized dSPE cleanup significantly minimized the matrix effects. Recoveries at 10, 25 and 50 mu g/kg were within 60-120% with associated precision, RSD < 11%. (C) 2015 Elsevier Ltd. All rights reserved.
机译:本文报道了一种选择性和灵敏的方法,用于多残留测定高脂肪鱼基质中的119种化学残留物,包括农药和多环芳烃(PAH)。新颖的样品制备方法涉及在己烷(2 mL)和剩余的水层进行三相分配后,从均质的鱼肉(5 g)在乙腈(15 mL,1%乙酸)中提取目标分析物。抽吸乙腈层的等分试样(1.5 mL),进行两步分散固相萃取(dSPE)净化,最后通过气相色谱质谱联用选定的反应监测器(GC-MS / MS)估算残留物。通过GC和四极杆飞行时间MS根据共混物的准确质量进行鉴定。在萃取过程中添加己烷和优化的dSPE净化可最大程度地降低基质效应。 10、25和50μg/ kg的回收率在60-120%之内,并且相关精度RSD <11%。 (C)2015 Elsevier Ltd.保留所有权利。

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