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建立了左氧氟沙星制剂中微量杂质的LC-MS/MS定量及筛查方法,方法学考察表明该方法快速、灵敏度高和专属性强。利用该方法对19个厂家市售左氧氟沙星药物制剂中的杂质进行检测和质量评价。上述样品中超过杂质限度的杂质共检出5种,且不同厂家制剂中的杂质含量差异较大,仅3个厂家制剂中杂质的含量均低于0.01%。左氧氟沙星的N4’-甲基季铵类杂质在左氧氟沙星制剂中首次检出。结合杂质来源,认为左氧氟沙星药物制剂中杂质水平的差异与原料药、制剂工艺参数的控制及运输储藏的环境有着密切关系。该方法能专属、灵敏和全面地检测药物制剂中的杂质,为客观评价制剂质量及质量控制提供了高效的分析手段,所检出杂质种类及含量水平能客观地反映左氧氟沙星制剂的质量。
The LC-MS / MS method for quantification and screening of trace impurities in levofloxacin preparations was established. The methodological study showed that the method was rapid, sensitive and specific. The method was applied to the detection and quality evaluation of the impurities in 19 pharmaceutical manufacturers of levofloxacin on the market. Five impurities were detected in the sample above the impurity limit, and the content of impurities in different manufacturers was quite different. Only three manufacturers contained less than 0.01% impurities. Levofloxacin N4’-methyl quaternary ammonium impurities in levofloxacin preparations for the first time detected. According to the sources of impurities, it is considered that the difference of impurity level in the levofloxacin drug preparation is closely related to the control of raw material medicine, preparation process parameters and the environment for transportation and storage. The method can detect the impurities in pharmaceutical preparations exclusively, sensitively and comprehensively, and provides an efficient analytical method for objectively evaluating preparation quality and quality control. The types and levels of impurities detected can objectively reflect the quality of the preparation of levofloxacin.