越鞠保和丸中5-羟甲基糠醛的限量检查  

Limit test for 5-hydroxymethylfurfural in Yueju Baohe pills

作　　者：牛辰瑾 安劼 邱铄雯 曲佳 NIU Chenjin;AN Jie;QIU Shuowen;QU Jia(Tianjin Institute for Drug Control,Tianjin 300070,China;Wuqing Branch of Tianjin Institute for Drug Control,Wuqing 301700,China;Tianjin Pharmaceutical Da Rentang Group Corporation Limited Traditional Chinese Pharmacy Research Institute,Tianjin 300457,China)

机构地区：[1]天津市药品检验研究院,天津300070 [2]天津市药品检验研究院武清药品检验所,天津武清301700 [3]津药达仁堂集团股份有限公司中药研究院,天津300457

出　　处：《中国药品标准》2024年第1期55-61,共7页Drug Standards of China

基　　金：国家药品监督管理局中国药品监管科学行动计划重点项目(NMPAJGKX-2023-079)。

摘　　要：目的:建立越鞠保和丸中5-羟甲基糠醛限量检查方法。方法:采用HPLC法,使用Zafex Acutfex PW-C_(18)(250 mm×4.6 mm,5μm)色谱柱;流动相为乙腈-0.1%甲酸水(2∶98);流速:1.0 mL•min^(-1);柱温:40℃;检测波长:284 nm。结果:5-羟甲基糠醛浓度在0.4919~122.98μg•mL^(-1)范围内,r=1.000,线性关系良好,方法平均回收率为97.99%,RSD为0.61%,精密度、重复性等试验结果均符合方法学测定要求。按照拟定限度要求,65批样品共17批不符合规定,不合格率26.15%。结论:建立的方法适用于越鞠保和丸中5-羟甲基糠醛的限度检查,抽样结果表明65批次样品中5-羟甲基糠醛含量差异较大。有必要对其限度进行控制。Objective:To establish an HPLC method to detect the limit of 5-hydroxymethylfurfural in Yueju Baohe pills.Methods:A Zafex Acutfex PW-C_(18) column(4.6 mm×250 mm,5μm)was adopted with mobile phase consisted of acetonitrile-0.1%formic acid aqueous solution(2∶98)at the flow rate of 1.0 mL•min^(-1).The column temperature was 40℃and the detective wavelength was set at 284 nm.Results:The linear range of 5-hydroxymethylfurfural was 0.4919-122.98μg•mL^(-1)(r=1.000).The average recovery(n=6)was 97.99%with RSD 0.61%.All of the RSDs for precision,repeatability and stability met the methodological requirements.According to the proposed limit,17 of the 65 batches of samples did not meet the requirements,and the failure rate was 26.15%.Conclusion:The established method is suitable for the limit test of 5-hydroxymethylfurfural in Yueju Baohe pills.There was a significant difference in the content of 65 batches of samples.It is necessary to investigate the limit of 5-hydroxymethylfurfural in Yueju Baohe pills.

关 键 词：越鞠保和丸 5-羟甲基糠醛 限度检查 高效液相色谱法 统计分析 质量控制 

分 类 号：R921.2[医药卫生—药学]