Simultaneous Determination of 69 Pesticide Residues in Coffee by Gas Chromatography-Mass Spectrometry

文献类型： 外文期刊

第一作者： Yang, Xin

作者： Yang, Xin;Xu, D. C.;Qiu, J. W.;Ma, Ying;Cui, J.;Yang, Xin;Wang, Jing

作者机构：

关键词： Pesticides;Multi-residue Analysis;Coffee;GPC;SPE;GC-MS

期刊名称：FOOD ANALYTICAL METHODS （ 影响因子：3.366； 五年影响因子：3.07 ）

ISSN： 1936-9751

年卷期： 2011 年 4 卷 2 期

页码：

收录情况： SCI

摘要： A method using gel permeation chromatography (GPC) combined with solid-phase extraction (SPE) cleanup followed by gas chromatography-mass spectrometry (GC-MS) has been established for quantitative determination of 69 pesticide residues in coffee. Based on an appraisal of the characteristics of GC-MS, validation experiments were conducted for 69 pesticides. In the method, 2.0 g samples were mixed with 5 ml water and 1 g sodium chloride and extracted with 5 ml of ethyl acetate by blender homogenization, centrifugation, and filtration. Evaporation was conducted and the sample was injected into a 250 mm x 10 mm S-X3 GPC column, with ethyl acetate-n-hexane (1:2 v/v) as the mobile phase at a flow rate of 3 ml/min. The 4-15 min fraction was collected for the SPE cleanup, which was Envi-Carb SPE cartridge coupled with NH2-LC SPE cartridge with acetone-ethyl acetate (2:5 v/v) as the eluted solvent. The eluents were collected and then evaporated to dryness, which was redissolved in 0.5 ml ethyl acetate for GC-MS analysis. For the 69 pesticides determined by GC-MS, the portions collected from GPC were concentrated to 0.5 ml and exchanged with 5 ml n-hexane. In the linear range of each pesticide, the correlation coefficient was R (2) a parts per thousand yenaEuro parts per thousand 0.99. At the low, medium, and high fortification levels of 0.05-1.0 mg/kg, recoveries fell within 60-120%. The relative standard deviation was between 1.3% and 22.3% for all 69 pesticides. The limits of detection for the method were 10 mu g/kg to 150 mu g/kg, depending on each pesticide.

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