高效液相色谱-串联质谱法测定蜂胶中的氯霉素

摘要

A method for the determination of chloramphenicol in propolis was developed by high performance liquid chromatography-tandem mass spectrometry. The flavones were removed with lead acetate solution after the extraction of the sample with water. The extract was cleaned up by liquid-liquid extraction. Internal standard method was used for quantitative analysis. The linear range was 0.05 - 2.0μg/L and the correlation coefficient ( r2 ) was 0. 999 6. The limit of detection (LOD, S/N = 3) and limit of quantitation (LOQ, S/N = 10) were 0. 1 μg/kg and 0. 3 μg/kg, respectively. The recoveries ranged from 70. 1% to 94.0% while the intra-day precision lower than 10% and inter-day precision lower than 15%. The method reduced the interference by removing most of the flavones and was suitable for the determination of chloramphenicol in propolis.%建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定蜂胶中氯霉素残留的方法.样品用水提取后,以醋酸铅溶液作为沉淀剂除去样品中的大部分黄酮类成分,用液-液萃取的方式提取样品中的氯霉素残留,最后以HPLC-MS/MS对样品进行定性、定量分析.该方法采用内标法定量,线性范围为0.05 ～2.0 μg/L,相关系数为0.999 6；方法的检出限(以信噪比(S/N)为3计)和定量限(以S/N=10计)分别为0.1μg/kg和0.3μg/kg；回收率范围为70.1％ ～ 94.0％,日内精密度小于10％,日间精密度在15.0％以下.该方法简便快捷,能除去蜂胶中的大部分黄酮类成分,减少了干扰,可以用于蜂胶中氯霉素残留的测定.