HPLC-ELSD法测定龙泽熊胆胶囊中牛磺熊去氧胆酸和牛磺鹅去氧胆酸的含量  

Determination of taursodeoxycholic acid and taurchenodeoxycholic acid in Longze Xiongdan capsules by HPLC-ELSD

作　　者：乔莉[1] 陈正东 陈馥[1] 简淑仪 黄俊忠[1] 黄悠雯 刘潇潇[1] QIAO Li;CHEN Zhengdong;CHEN Fu;JIAN Shuyi;HUANG Junzhong;HUANG Youwen;LIU Xiaoxiao(Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《中国药品标准》2024年第1期76-81,共6页Drug Standards of China

基　　金：广东省中医药局课题(20221056)。

摘　　要：目的:以牛磺熊去氧胆酸和牛磺鹅去氧胆酸为指标,建立龙泽熊胆胶囊中熊胆粉的含量测定方法。方法:采用高效液相色谱串联蒸发光检测器,色谱柱为ChromCore AQ C 18(4.6 mm×250 mm,5μm),乙腈(A)-5 mmol•L^(-1)醋酸铵溶液(B)为流动相,梯度洗脱(0~40 min,25%A;40~50 min,25%A→29%A;50~80 min,29%A;80~100 min,29%A→40%A),流速1.0 mL•min^(-1),柱温30℃,ELSD漂移管温度110℃,氮流量2.5L•min^(-1)。结果:牛磺熊去氧胆酸进样量在1.069~9.57μg内、牛磺鹅去氧胆酸进样量在0.74046~7.40464μg内,进样量的对数与峰面积的对数呈良好的线性关系;仪器精密度、重复性、稳定性试验的RSD<2.0%;经低、中、高3个浓度的准确度试验考察,牛磺熊去氧胆酸的回收率为95.2%~97.7%,牛磺鹅去氧胆酸的回收率为91.9%~95.9%。测定样品42批次,牛磺熊去氧胆酸和牛磺鹅去氧胆酸的含量分别为0.18~0.43、0.10~0.44 mg•粒^(-1)。结论:本法适用于龙泽熊胆胶囊中熊胆粉的质量控制,可为完善龙泽熊胆胶囊的质量标准提供科学的依据。Objective:To establish a method for determining the content of bear bile powder in Longze Xiongdan capsules with taursodeoxycholic acid(TUDCA)and taurchenodeoxycholic acid(TCDCA)as indexes.Methods:HPLC series evaporation photodetector was adopted on Chrom Core AQ C 18 column(4.6 mm×250 mm,5μm),with the mobile phase comprising of acetonitrile(A)and 5 mmol•L^(-1) ammonium acetate solution(B)in a gradient elution(0-40 min,25%A;40-50 min,25%A→29%A;50-80 min,29%A;80-100 min,29%A→40%A)at the flow rate of 1.0 mL•min^(-1).The column temperature was 30℃.The ELSD was used,of which the drift tube temperature was 110℃and the flow rate of carrier gas(N 2)was 2.5 L•min^(-1).Results:In the ranges of 1.069-9.57μg and 0.74046-7.40464μg,logarithms of the injected amount of TUDCA and TCDCA presented good linear relationships with logarithms of the peak area,respectively.The RSDs of precision,repeatability and stability tests were all lower than 2.0%.At three concentration levels the recoveries of TUDCA and TCDCA were 95.2%-97.7%and 91.9%-95.9%,respectively.Samples of 42 batches showed that the contents of TUDCA and TCDCA were 0.18-0.43 and 0.10-0.44 mg•granule^(-1),respectively.Conclusion:This method can be used for the quality control of bear bile powder in Longze Xiongdan capsules,thus provides a scientific basis for improving its quality standard.

关 键 词：高效液相色谱-蒸发光散射检测器 龙泽熊胆胶囊 熊胆粉 牛磺熊去氧胆酸 牛磺鹅去氧胆酸 

分 类 号：R921.2[医药卫生—药学]