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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0.05～2.0μg/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。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) was developed for the determination of chloramphenicol residues in propolis. After the sample was extracted with water, most of the flavonoids in the sample were removed by using lead acetate solution as precipitant, and the residuals of chloramphenicol in samples were extracted by liquid-liquid extraction. Finally, the samples were qualitative and quantitative by HPLC-MS / MS analysis. The method was quantified by internal standard method with a linear range of 0.05-2.0 μg / L and a correlation coefficient of 0.999 6. The detection limit (S / N ratio was 3) and the limit of quantitation (S / N) N = 10) were 0.1μg / kg and 0.3μg / kg respectively. The recoveries ranged from 70.1% to 94.0%. The intra-day precision was less than 10% and the intra-day precision was less than 15.0%. The method is simple and quick, can remove most of the flavonoids in the propolis, reduces the interference and can be used for the determination of chloramphenicol residues in the propolis.