对乙酰氨基酚栓国家药品评价性抽检工作中发现的问题及解决方案  

Quality related problems and solutions of paracetamol suppositories in national drug sampling and inspection

作　　者：窦艳丽 张乃斌 陈真 李琳 杨书娟 王雪 张雷 徐玉文 DOU Yan-li;ZHANG Nai-bin;CHEN Zhen;LI Lin;YANG Shu-juan;WANG Xue;ZHANG Lei;XU Yu-wen(Shandong Institute for Food and Drug Control,China,NMPA Key Laboratory for Research and Evaluation of Generic Drups,Shandong Research Center of Engineering and Technology for Consistency Evaluation of Generic Drugs,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院,仿制药研究与评价重点实验室,山东省仿制药一致性评价工程技术研究中心,济南250101

出　　处：《药物分析杂志》2022年第3期531-536,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:基于对乙酰氨基酚栓国评工作中发现的问题,建立新的对乙酰氨基酚栓的含量测定方法并开展相关探索性研究。方法:采用Agilent C_(18) plus(250 mm×4.6 mm,5μm)色谱柱,对对乙酰氨基酚栓的含量进行测定,以0.05 mol·L^(-1)醋酸铵溶液-甲醇(85∶15)为流动相,流速为1 mL·min^(-1),检测波长257 nm。结果:对乙酰氨基酚在1.5~300μg·mL^(-1)范围内呈现良好的线性关系(r=1.000),平均回收率(n=9)为100.1%、精密度低至0.44%。建立了新的对乙酰氨基酚栓含量测定方法,解决了原方法样品制备困难、实验方法精密度差的问题。同时在质量标准中增加了含量均匀度检查项,有效控制了产品含量的均一性。结论:本方法专属性强,结果准确度高,重复性好,方法耐用性良好,很好的解决了国评实验中对乙酰氨基酚含量测定精密度及准确度差的问题,为有效控制该栓剂的质量提供一种准确实用的手段。Objective:To establish an HPLC method to determine the assay of paracetamol suppositories and carry out the related exploratory research based on the problems found in the national evaluation sampling inspection.Methods:Agilent C_(18) plus(250 mm×4.6 mm,5μm)column was used to determine the assay of paracetamol suppository.The mobile phase was 0.05 mol·L^(-1) ammonium acetate-methanol(85∶15),the flow rate was 1 mL·min^(-1),and the detection wavelength was 257 nm.Results:The linear range of paracetamol was 1.5-300μg·mL^(-1)(r=1.000),and the average recovery was 100.1%,precision was 0.44%.A new method for the determination of paracetamol suppositories content was established,which solved the problems of sample preparation and precision of the original method.Meanwhile,the content uniformity was added in the quality standard,which assures the uniformity of product content.Conclusion:The method has strong specificity,high accuracy,good reproducibility and good durability.The problem of poor precision and accuracy in the determination ofparacetamol content was well solved and provides an accurate and practical method for the quality control of the suppository.

关 键 词：对乙酰氨基酚栓 国家药品评价性抽检 含量测定 含量均匀度 高效液相色谱法 混悬型 药物分布 

分 类 号：R917[医药卫生—药物分析学]