水产品中氯霉素检测条件的优化

Optimization of detection conditions of chloramphenicol in aquatic products

中文关键词:  液相色谱串联质谱法  氯霉素  加工水产品

英文关键词:high performance liquid chromatography-tandem mass spectrometry  chloramphenicol  processed aquatic products

中文摘要:

      目的 建立液相色谱串联质谱法测定加工水产品中的氯霉素, 并对提取溶剂、净化条件、流动相进行了优化。方法 样品采用乙酸乙酯提取, HLB固相萃取柱净化, C18色谱柱分离, ESI源负离子模式对氯霉素进行检测。结果 氯霉素在0.1~10 μg/kg范围内线性关系良好, 相关系数为0.999, 在基质样品中添加0.1、0.2和10.0 μg/kg 3个水平药物, 其回收率在95.0%~103.2%之间, 相对标准偏差3.72%~6.85%, 方法检测限为0.1 μg/kg. 结论 该方法可靠、稳定, 可满足加工水产品中氯霉素残留检测与确证需要。

英文摘要:

      Objective To establish a method for the determination of chloramphenicol in aquatic products by high performance liquid chromatography- tandem mass spectrometry, and to optimize the sample pretreatment such as extraction, cleanup and mobile phase. Methods Samples were extracted with ethyl acetate, cleaned up by the Oasis HLB SPE cartridges and collected by the C18 chromatographic column. Finally, the chloramphenicol was detected in the ESI negative ion mode. Results The linear ranges were 0.1?10 μg/kg and the correlation coefficients were all above 0.99. The recoveries of chloramphenicol in aquatic products at the spiked levels of 0.1, 0.2 and 10 μg/kg were in ranges of 95.0%?103.2%. The relative standard deviations were 3.72%~6.85%, and the limit of detection was 0.1 μg/kg. Conclusion The method is reliable and stable, which can meet the requirements for the determination of chloramphenicol in aquatic products.