九华痔疮栓中大黄素和大黄酚定量方法研究
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摘要
目的九华痔疮栓收载于《卫生部药品标准》中药成方制剂第十八册,方中大黄为君药,主要的活性成分是蒽醌类成分,而质量标准未对产品中大黄蒽醌类成分进行质量控制。为了进一步完善九华痔疮栓的质量标准,研究建立HPLC法测定九华痔疮栓中大黄素和大黄酚的含量。方法采用Wondasil C18(4.6 mm×250 mm,5μm)色谱柱;以甲醇-0.1%磷酸溶液(70∶30)为流动相;流速1.0 mL/min;检测波长254 nm;柱温30℃。结果大黄素在0.008288～0.248 64μg范围内呈良好的线性关系(r=0.999 99),平均回收率(n=6)为99.6%;大黄酚在0.021 8～0.654μg范围内呈良好的线性关系(r=0.999 98),平均回收率(n=6)为95.4%。结论该定量方法简便、准确,重复性好,可作为九华痔疮栓的质量控制方法。
Objective Jiuhua Zhichuang suppositories was included in the 18 th volume of TCM prescription preparation of ministry of health drug standard, Rhubarb is the king of the prescription, and the main active ingredient is anthraquinone.The quality standard did not control the anthraquinones in rhubarb. To further improve the quality standard of jiuhua Zhichuang suppositories,HPLC method was established to determine the content of Emodin and Chrysophanol in jiuhua Zhichuang suppositories.Methods The analytical column Wondasil C18 column(4.6 mm×250 mm, 5 μm) was adopted, and the mobile phase was methanol-0.1%phosphoric(70:30) at the flow rate of 1.0 mL/min, and the detecting wavelength was 254 nm, the column temperature was 30℃. Results Emodin curves were linear in the range of 0.008 288～0.24 864 μg(r=0.999 99),and the average recovery(n=6) was 99.6%; Chrysophanol curves were linear in the range of 0.0218～0.654 μg(r=0.999 98), and the average recovery(n=6) was 95.4%. Conclusion The quantitative method is simple, accurate and reproducible, and can be used for quality control of Jiuhua Zhichuang Suppositories.
Objective Jiuhua Zhichuang suppositories was included in the 18 th volume of TCM prescription preparation of ministry of health drug standard, Rhubarb is the king of the prescription, and the main active ingredient is anthraquinone.The quality standard did not control the anthraquinones in rhubarb. To further improve the quality standard of jiuhua Zhichuang suppositories,HPLC method was established to determine the content of Emodin and Chrysophanol in jiuhua Zhichuang suppositories.Methods The analytical column Wondasil C18 column(4.6 mm×250 mm, 5 μm) was adopted, and the mobile phase was methanol-0.1%phosphoric(70:30) at the flow rate of 1.0 mL/min, and the detecting wavelength was 254 nm, the column temperature was 30℃. Results Emodin curves were linear in the range of 0.008 288～0.24 864 μg(r=0.999 99),and the average recovery(n=6) was 99.6%; Chrysophanol curves were linear in the range of 0.0218～0.654 μg(r=0.999 98), and the average recovery(n=6) was 95.4%. Conclusion The quantitative method is simple, accurate and reproducible, and can be used for quality control of Jiuhua Zhichuang Suppositories.
引文
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[2]袁向飞,谢俊木子,谭晓华.大黄及其有效成分抗肿瘤的研究进展[J].中国中西医结合外科杂志,2018,24(3):363-366.
[3]常志惠,胡军华,万亚菲,等.一测多评法同时测定保肾乙丸中5种蒽醌类成分的含量[J].中国药房,2016,36(27):5156-5159.
[4]刘远平,陈粟.不同产地药用大黄中5种游离蒽醌的含量测定[J].亚太传统医药,2016,12(5):42-44.
[5]杨滢.大黄药效成分及其药理活性研究进展[J].中国临床研究,2018,10(5):148-150.
[6]Liu S,Wang J,Shao T,et al. The natural agent rhein inducesβ-catenin degradation and tumour growth arrest[J]. J Cell Mol Med,2018,22(1):589-599.
[7]国家药典委员会.中华人民共和国药典一部[S]. 2015年版.北京:中国医药科技出版社,2015:23.
[8]杨娟艳,王珍珍,茅向军,等. HPLC法比较3种土大黄中游离蒽醌和总蒽醌的含量[J].药物分析杂志,2017,37(4):615-623.
[9]廖李奎,贾少谦.四味雪莲花颗粒中大黄酚、大黄素含量测定方法[J].中医学报,2016,31(8):1153-1155.
[10]何盛江,聂阳,陈刚,等.HPLC法同时测定不同产地羊蹄药材中大黄素、大黄酚、大黄素甲醚的含量[J].中药材,2016,33(27):4719-4721.
[11]赵丽君. HPLC法同时测定牛黄上清丸中4种葱醒类化合物的含量[J].中国药房,2016,27(3):402-404.
[12]李子君,牟晓崟. HPLC法同时测定肿痛外擦酊中大黄酸、大黄素、芦荟大黄素、大黄酚、大黄素甲醚的含量[J].海峡药学,2017,29(9):46-48.
[13]王迅,邹恺平,周琴妹.等.小儿退热合剂定性定量研究[J].江苏中医药,2018,50(10):68-71.