猪胆粉中牛磺猪去氧胆酸测定方法的改进  

Improvement of Determination of Taurohyodeoxycholic Acid in Suis Fellts Pulvis

作　　者：张平 张健敏 杨平荣 杨莉 刘志荣 王晓琳[3] ZHANG Ping;ZHANG Jian-Min;YANG Ping-rong;YANG Li;LIU Zhi-rong;WANG Xiao-lin(Gansu Institute for Drug Control,Gansu Lanzhou 730070,China;Gansu Provincial Traditional Chinese Medicine Inspection and Testing Technology Engineering Laboratory,Gansu Lanzhou 730070,China;Gansu Provincial Hospital of Traditional Chinese Medicine,Gansu Lanzhou 730070,China)

机构地区：[1]甘肃省药品检验研究院,甘肃兰州730070 [2]甘肃省中藏药检验检测技术工程实验室,甘肃兰州730070 [3]甘肃省中医院,甘肃兰州730050

出　　处：《中国药物评价》2020年第4期273-275,共3页Chinese Journal of Drug Evaluation

摘　　要：目的:改进猪胆粉药材牛磺猪去氧胆酸的色谱条件,解决原方法不能使被检测成分完全分离的问题。方法:将原方法由甲醇-0.03 mol·L^-1磷酸二氢钠溶液(70∶30)(用磷酸调节pH值为4.4)改为乙腈-0.03 mol·L^-1磷酸二氢钠,梯度洗脱;体积流量1.0 mL·min^-1;柱温30℃;检测波长200 nm。结果:牛磺猪去氧胆酸在0.5097~10.1940μg(r=0.9999)范围内呈良好的线性关系,平均加样回收率在98.6%~102.8%间,RSD均小于1.70%。在45 min内达到基线分离,该方法可以准确对猪胆粉中牛磺猪去氧胆酸进行定性定量。结论:该方法改善了原方法不能达到分离被测成分的问题,检测结果稳定、可靠,重现性好,适用于猪胆粉的质量控制,可为2015版《中国药典》中猪胆粉药材测定方法的改进提供参考。Objective:To improve the chromatographic conditions of taurohyodeoxycholic acid of Suis fellts pulvis drug and to solve the problem that the original method could not completely separate the detected components.Method:The original method was changed from methanol-0.03 mol·L^-1 sodium dihydrogen phosphate solution(70∶30)(adjusted pH to 4.4 by phosphoric acid)to acetonitrile-0.03 mol·L^-1 sodium dihydrogen phosphate,gradient elution.The flow rate was 1.0 mL·min^-1.The column temperature was 30℃.The detection wavelength was 200 nm.Results:Taurohyodeoxycholic acid showed a good linear relationship in the range of 0.5097-10.1940μg(r=0.9999).The average sample recovery was between 98.6%-102.8%,and the RSDs were less than 1.70%.Baseline separation was achieved within 45 min.This method can accurately quantify taurohyodeoxycholic acid in Suis fellts pulvis.Conclusion:This method improves the problem that the original method cannot achieve the separation of the tested components.The test results are stable,reliable,and reproducible.It is suitable for the quality control of Suis fellts pulvis.It can provide reference for the improvement of the determination method of Suis fellts Pulvis in Chinese Pharmacopoeia 2015.

关 键 词：猪胆粉 牛磺猪去氧胆酸 高效液相色谱法 

分 类 号：R931.74[医药卫生—生药学] R284.1[医药卫生—药学]