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目的:评价美国药典肝素中残留蛋白质检测新方法的适用性,收集多批原料药检测数据以便确定适合的限度。方法:采用Lowry法及加入去除干扰物质的前处理过程的Lowry法对美国药典委员会提供的2个测试样品及2个国内生产厂家的10批肝素钠原料药进行了检测。结果:中检院2个测试样品结果符合USP要求,提交的实验数据全部被采纳。全球共14个实验室提交了141批肝素钠原料药结果,除1个实验室不符合系统适用性要求,数据未被采纳外,其余原料蛋白含量均小于0.1%。结论:美国药典新的肝素中残留蛋白质检测方法及限度是可行的,对预实验蛋白质含量超过0.1%的样品,进行去干扰物质预处理,将残留蛋白质限度从“不得过1.0%”提高至“不得过0.1%”。
OBJECTIVES: To evaluate the applicability of the new method for the detection of residual proteins in the heparin of the United States Pharmacopeia and to collect data from multiple batches of APIs in order to determine the appropriate limits. Methods: Two test samples provided by the USP and two batches of 10 heparin sodium APIs from domestic manufacturers were tested by Lowry method and Lowry method by adding pretreatment to remove interfering substances. Results: The results of the two test samples of the CIQ meet the requirements of the USP. All the submitted experimental data were adopted. 141 batches of heparin sodium APIs were submitted by 14 laboratories worldwide. All but one laboratory did not meet the system suitability requirements and the data were not accepted. All other raw protein contents were less than 0.1%. CONCLUSION: The method and limit of detection of new protein in heparin of the United States Pharmacopoeia are feasible. Pretreatment of samples with pre-experimental protein content more than 0.1% can improve the limit of residual protein from 1.0% To “must not exceed 0.1% ”.