Determination of organochlorine pesticides in propolis by gas chromatography-electron capture detection using double column series solid-phase extraction

文献类型: 外文期刊

第一作者: Chen, Fang

作者: Chen, Fang;Chen, Lanzhen;Zhou, Jinhui;Xue, Xiaofeng;Zhao, Jing;Wang, Qiang

作者机构:

关键词: Propolis;Organochlorine pesticides (OCPs);Solid-phase extraction (SPE);Gas chromatography-electron capture detection (GC-ECD);MASS-SPECTROMETRY;MULTIRESIDUE METHOD;RESIDUES;CLEANUP;MICROEXTRACTION;CONTAMINANTS;VEGETABLES;BEESWAX;FRUITS;HONEY

期刊名称:ANALYTICAL AND BIOANALYTICAL CHEMISTRY ( 影响因子:4.142; 五年影响因子:3.863 )

ISSN:

年卷期:

页码:

收录情况: SCI

摘要: A rapid and reliable method was developed and applied for the simultaneous determination of 17 organochlorine pesticides (OCPs) in propolis. After extraction with hexane and acetone (1:1, v/v), four sorbents (florisil, silica, graphitized carbon, and tandem graphitized carbon plus florisil) were assayed for the clean-up step. The elution solvents hexane and ethyl acetate (1:1, v/v), hexane and dichloromethane (3:7, v/v), and ethyl acetate and hexane (2: 8, v/v) were studied. The results showed that the combination of the tandem graphitized carbon and florisil cartridge with the elution solvent of 6mL of ethyl acetate and hexane (2:8, v/v), which was capable of eliminating matrix interference and providing colorless eluates, was the most efficient clean-up procedure for propolis extracts when testing for OCPs. The analytical technique employed was gas chromatography with electron capture detection (GC-ECD). The correlation coefficients from linear regression for the analyzed concentrations (5 similar to 100 mu g/kg) were >0.9961. The limits of detection (LODs) varied between 0.8 mu g/kg for 4,4'-DDE and 11.4 mu g/kg for endosulfan II, and the limits of quantitation (LOQs) ranged from 2.6 to 38.1 mu g/kg. The average recoveries varied between 62.6 and 109.6%. Relative standard deviations (RSD%) ranged from 0.8 to 9.4%. Sample analysis indicated that 4,4'-DDE was detected more often in propolis than other pesticides, such as beta-HCH, delta-HCH and heptachlor.

分类号: O65

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