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Determination of chloramphenicol in propolis in China markets by liquid chromatography/tandem mass spectrometry

机译:液相色谱/串联质谱法测定中国蜂胶中的氯霉素

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A method based on high performance liquid chromatography — tandem mass spectrometry was established for the determination of chloramphenicol (CAP) residues in propolis. The propolis samples were dissolved with 1 M sodium hydroxide (NaOH), acidified with 5% perchloric acid (HClO4), then were adjusted to pH=10 with 1M NaOH. The solutions were extracted with ethyl acetate, followed by treatment with n-hexane for defatting. D5-chloramphenicol (CAP-D5) was utilized as internal standard. The results showed that linearity of the method was good with correlation coefficients (R2) of 0. 9999 in the range of 0.2 to 10μg/kg. The detection limit was 0.05μg/kg. The recoveries varied from 89.0% to 94.3% with the relative standard deviation (RSD) from 5.78% to 10.25% Using this method, the concentrations of CAP in 8 propolis samples collected in China markets were determined with content ranged from <0.05 to 0.95μg/kg. The method is sensitive, reproducible and suitable for the determination of CAP residues in propolis.
机译:建立了一种基于高效液相色谱-串联质谱法测定蜂胶中氯霉素(CAP)残留量的方法。蜂胶样品用1 M氢氧化钠(NaOH)溶解,用5%高氯酸(HClO 4 )酸化,然后用1M NaOH调节至pH = 10。溶液用乙酸乙酯萃取,然后用正己烷处理脱脂。 D5-氯霉素(CAP-D5)被用作内标。结果表明,该方法的线性度良好,相关系数(R 2 )为0. 9999,范围为0.2至10μg/ kg。检出限为0.05μg/ kg。回收率从89.0%到94.3%,相对标准偏差(RSD)从5.78%到10.25%。使用此方法,测定了中国市场上采集的8种蜂胶样品中CAP的浓度,含量在<0.05至0.95μg之间。 /公斤。该方法灵敏,可重现,适用于测定蜂胶中的CAP残留量。

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