Determination of pesticides in seaweeds by pressurized liquid extraction and programmed temperature vaporization-based large volume injection-gas chromatography-tandem mass spectrometry

被引:36
|
作者
Garcia-Rodriguez, D. [1 ]
Carro-Diaz, A. M. [1 ]
Lorenzo-Ferreira, R. A. [1 ]
Cela-Torrijos, R. [1 ]
机构
[1] Univ Santiago de Compostela, Dpto Quim Analit Nutr & Bromatol, Fac Quim, IIAA, Santiago De Compostela 15782, Spain
关键词
Pressurized liquid extraction; Large volume injection-programmed temperature vaporization; GC-MS/MS; Pyrethroid; Organophosphorus pesticides; Carbaryl; Seaweed; SOLID-PHASE EXTRACTION; MICROWAVE-ASSISTED EXTRACTION; POLYCYCLIC AROMATIC-HYDROCARBONS; ORGANOCHLORINE PESTICIDES; ORGANOPHOSPHORUS PESTICIDES; PYRETHROID INSECTICIDES; PARTICULATE SAMPLES; MULTIRESIDUE METHOD; WATER EXTRACTION; ELECTRON-CAPTURE;
D O I
10.1016/j.chroma.2010.02.061
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A rapid method for the simultaneous identification and quantification of pesticide residues in edible seaweed has been developed. Target analytes were three pyrethroid, a carbamate and two organophosphorus pesticides. The procedure consists of a pressurized liquid extraction (PLE) with integrated clean-up, followed by gas chromatography coupled to tandem mass spectrometry. Five PLE parameters were investigated using a screening design: temperature, static extraction time, number of cycles, percent of flush volume and quantitative composition of the n-hexane/ethyl acetate extraction solvent. The effect of the in-cell clean-up with Florisil (R) and graphitized carbon black adsorbents was investigated using a Doehlert response surface design. Large volumes of sample extracts were injected using a programmed-temperature vaporizer (PTV-LVI) to improve both sensitivity and selectivity of measurements. Quantification was carried by the internal standard method with surrogate deuterated standards. The method showed excellent linearity (R-2 > 0.999) and precision (relative standard deviation, RSD <= 8%) for all compounds, with detection limits ranging from 0.3 pg g(-1) for chlorpyrifos-ethyl, to 3.0 pg g(-1) for carbaryl (23.1 pg g(-1) for deltamethrin). Recoveries in real seaweed samples were within the range 82-108%. The method was satisfactory validated for the analysis of wild and cultivated edible seaweeds. The presence of pyrethroid and organophosphorus pesticides in some of the samples was evidenced. (C) 2010 Elsevier B.V. All rights reserved.
引用
收藏
页码:2940 / 2949
页数:10
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