龙泽熊胆胶囊质量标准提升研究  

Improvement of Quality Standard for Longze Xiongdan Capsules

作　　者：苏章轩 刘潇潇[1] 张恺东 陆佳 SU Zhangxuan;LIU Xiaoxiao;ZHANG Kaidong;LU Jia(Guangdong Institute for Drug Control,Guangzhou,Guangdong,China 510180)

机构地区：[1]广东省药品检验所,广东广州510180

出　　处：《中国药业》2024年第6期77-81,共5页China Pharmaceuticals

基　　金：广东省药品监督管理局科技创新项目[2023YDZ03]。

摘　　要：目的提升龙泽熊胆胶囊的质量标准。方法采用薄层色谱(TLC)法对防风药材中的升麻素和5-O-甲基维斯阿米醇进行定性鉴别,并进行耐用性考察。采用高效液相色谱法同时测定制剂中上述2种成分的含量,色谱柱为Wondasil C18柱(200 mm×4.6 mm,5μm),流动相为乙腈-水(梯度洗脱),流速为0.8 mL/min,检测波长为254 nm,柱温为30℃,进样量为20μL。结果TLC图斑点清晰、分离度好,且阴性对照无干扰。升麻素和5-O-甲基维斯阿米醇进样量分别在0.051~1.020μg、0.025~0.499μg范围内与峰面积线性关系良好(R^(2)=1.000);检测限均为0.1μg/mL,定量限均为0.3μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为96.20%和91.40%,RSD分别为1.09%和1.89%(n=6)。结论所建立的方法专属性强,重复性、耐用性好,结果稳定,可为龙泽熊胆胶囊的质量控制提供参考。Objective To improve the quality standard of Longze Xiongdan Capsules.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify the cimifugin and 5-O-methylvisamminol in Saposhnikoviae Radix,and the durability was investigated.High-performance liquid chromatography(HPLC)method was used to simultaneously determine the contents of the above two components in the preparation;the chromatographic column was Wondasil C18 column(200 mm×4.6 mm,5μm),the mobile phase was acetonitrile-water(gradient elution),the flow rate was 0.8 mL/min,the detection wavelength was 254 nm,the column temperature was 30℃,and the injection volume was 20μL.Results The TLC chromatograms had clear spots and good resolution,and the negative reference had no interference.The linear ranges of cimifugin and 5-O-methylvisamminol were 0.051-1.020μg,0.025-0.499μg(R^(2)=1.000)respectively.The limits of detection of the above two components were both 0.1μg/mg,and their limits of quantification were both 0.3μg/mL.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of the above two components were 96.20%,91.40%,with the RSDs of 1.09%,1.89%(n=6)respectively.Conclusion The established method is specific,repeatable,durable and stable,which can provide a reference for the quality control of Longze Xiongdan Capsules.

关 键 词：龙泽熊胆胶囊 防风 升麻素 5-O-甲基维斯阿米醇 薄层色谱法 高效液相色谱法 质量控制 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]