高效液相色谱-串联质谱法测定蜂胶中的氯霉素

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0.9996;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0.1 μg/kg和0.3 μg/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。

Determination of chloramphenicol in propolis by high performance liquid chromatography-tandem mass spectrometry

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 - 2.0 microg/L and the correlation coefficient (r2) was 0.9996. The limit of detection (LOD, S/N = 3) and limit of quantitation (LOQ, S/N = 10) were 0.1 microg/kg and 0.3 microg/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.