摘要
目的:建立控制局方至宝散中牛黄质量的分析方法,用于制剂中投料所用牛黄的品种及质量监控。方法:采用薄层检查法检测猪去氧胆酸成分;采用薄层扫描法对局方至宝散中牛黄的胆酸含量进行测定,展开剂为环己烷-乙酸乙酯-36%乙酸-甲醇(20∶25∶2∶3)上层溶液,展开2次;薄层板为硅胶G板,显色剂为10%硫酸乙醇溶液(V/V)1,05℃加热至斑点显色清晰;检测波长为460 nm;采用高效液相色谱法对局方至宝散中牛黄的胆红素含量进行测定,色谱柱为Kromasil-C18(150 mm×4.6 mm,5μm)柱,流动相为乙腈-1%冰乙酸溶液(95∶5,V/V),流速为1.0 ml/min,检测波长为450 nm。结果:薄层检查法中,猪去氧胆酸的最低检出量为0.04μg。薄层扫描法中,胆酸线性范围为25.1 mg/ml～502.0 mg/ml,相关系数为0.999,检出限为0.06μg;平均加标回收率为100.8%,RSD为1.64%。高效液相色谱法中,胆红素方法线性范围为1.22 mg/ml～61.0 mg/ml,相关系数为0.9999,检出限为0.002μg;平均加标回收率为99.0%,RSD为1.62%。结论:该法操作简便,结果准确可靠,应用性较广。
Objective：To establish a set of analytical methods for controling the quality of Calculus Bovis in the Jufang Zhibao Powder.The methods can be used to control the variety and quality of Calculus Bezoar materials used in Jufang Zhibao Powder.Methods：Thin-layer chromatography（TCL） was used to determine hyodeoxycholic acid and Thin-layer chromatography scanning（TLCS） method was used to determine cholic acid,the developer was the mixture of cyclohexane-ethyl acetate-36% acetic acid-methanol（20：25：2：3） upper solution.The TLC plate was silica gel G plate and the colour developing reagent was 10% solution of sulfuric acid in ethanol（V/V）.To heat at 105℃ to develop clearly,the detection wavelength was 460 nm.High performance liquid chromatography was used to determine bilirubin,Kromasil-C18（150 mm×4.6 mm,5 μm） was used as separation column with mobile phase of acetonitrile-1% glacial acetic acid solution（95：5,V/V） and flow rate of 1.0 ml/min.The detection wavelength was 450 nm.Results：The minimum detectable amount of hyodeoxycholic was 0.04 μg by TLC.In the system of TCLS,the linear range is 25.1 mg/ml～502.0 mg/ml with the correlation coefficient of 0.999 and the detection limit of 0.06 μg.The average recovery was 100.8% with RSD of 1.64%.For HPLC,the linear range of 1.22 mg/ml～61.0 mg/ml with the correlation coefficient of 0.9999 and the detection limit of 0.002 μg was obtained.The average recovery was 99.0% with RSD of 1.62%.Conclusion：The methods are simple and accurate with wide application.
出处
《中国卫生检验杂志》
CAS
2011年第8期1872-1874,1877,共4页
Chinese Journal of Health Laboratory Technology
基金
重大新药创制项目(2009ZX09308-004)
关键词
牛黄
局方至宝散
薄层检查法
薄层扫描法
高效液相色谱法
Calculus Bovis
Jufang Zhibao Powder
Thin-layer chromatography
TLCS
High performance liquid chromatography
作者简介
夏晶（1972-），女，在职研究生，副主任药师，主要从事天然药物、食品理化检验工作。
通讯联系人，E—mail：jishen2008@gmail．com
