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几种动物源性食品中氯霉素残留量的气相色谱双电子俘获检测

Determination of Chloramphenicol Residues in Animal-origin Food samples by Gas Chromatography with Double Electron Capture Detector

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【作者】 王建华梁成珠刘兴敏张艺兵林黎明

【Author】 WANG Jian_hua,LIANG Cheng_zhu,LIUXing_min,ZHANG Yi_bing,LIN Li_ming (Qingdao Exit&Entry Inspection and Quarantine Bureau,Qingdao266002,China)

【机构】 青岛出入境检验检疫局食品实验室青岛出入境检验检疫局食品实验室 山东青岛266002山东青岛266002山东青岛266002

【摘要】 研究了几种动物源性食品中氯霉素残留量的气相色谱测定方法;样品中氯霉素残留用乙酸乙酯提取,浓缩至干,溶于氯化钠溶液,用正己烷脱脂,水层再用乙酸乙酯提取,浓缩后用N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA)+1%三甲基氯硅烷(TMCS)衍生,用外标法定量;采用不同极性的色谱柱定性。当添加水平为0.3×10-9~10×10-9(w)时,回收率大于80%,相对标准偏差小于20%,线性相关系数r=0.999。

【Abstract】 A method for the determination of chloramphenicol residues in animal-origin food samples by gas chromatography(GC)with double electron capture detector is described.The sample pretreatment procedure inˉcludes extraction with ethyl acetate,evaporation of the extracts to dryness,dissolution of residues in aqueous sodium chloride solutions,extraction with n_hexane for the removal of fats,re_extraction of chloramphenicol into the ethyl acetate medium,and concentration of the ethyl acetate solution.The chloramphenicol in the concentratˉed ethyl acetate solution was finally derivatized with99%N,O_bis(trimethylsilyl)trifluoroacetamide(BSTFA)-1%trimethylchlorosilane(TMCS).Good repetitivity can be obtained with a RSD less than20%.The limit of detection is0.2μg/kg.At spiked levels of0.3×10 -9 ~10×10 -9 (w),the mean recovery exceeds80%.The linear correlation coefficient r equals to0.999.The method is cheap,rapid and sensitive,and can be applied to routine analysis.

  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2003年05期
  • 【分类号】O657.7
  • 【被引频次】24
  • 【下载频次】107
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