杜仲降压片质量标准的提高与优化  

Study on the quality standard of Duzhong Jiangya tablets

作　　者：孙慧珠 刘晓明 徐乐 王常顺 刘永利 SUN Hui-zhu;LIU Xiao-ming;XU Le;WANG Chang-shun;LIU Yong-li(Hebei Institute for Drug Control,Hebei Shijiazhuang 050011,China)

机构地区：[1]河北省药品检验研究院,石家庄050011

出　　处：《药物分析杂志》2020年第8期1514-1520,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会2015年标准提高项目(98)。

摘　　要：目的:完善杜仲降压片质量标准,提高其质量控制水平。方法:建立了以杜仲及钩藤对照药材为对照的薄层色谱鉴别方法,同时建立了高效液相色谱法同时测定迷迭香酸、黄芩苷、黄芩素的含量,采用Thermo Acclaim C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸为流动相进行梯度洗脱,流速1.0mL·min^-1,检测波长为330 nm。结果:薄层色谱鉴别方法专属性良好,斑点清晰。迷迭香酸、黄芩苷、黄芩素分别在进样量为0.049 92~0.898 6μg、0.677 6~3.388 0μg、0.083 50~0.453 6μg范围内线性关系良好,相关系数均为0.999 9;平均加样回收率在100.3%~102.6%范围内,RSD均小于1.3%。15批样品中3个待测成分分别在0.02~0.15,3.71~7.59,0.16~1.25 mg·片^-1范围内。结论:本研究建立的方法准确可靠,可为杜仲降压片的质量标准完善提供更为全面的科学依据。Objective:To improve the quality standard of Duzhong Jiangya tablets and improve its quality control level. Methods:TLC method for identification of Eucommiae Cortex and Uncariae Ramulus cum Uncis were established. The HPLC method for the determination of rosmarinic acid,baicalin and baicalein was developed and validated. The chromatographic separation was preformed on a Thermo Acclaim C18(4.6 mm×250 mm,5 μm)column with acetonitrile-0.1% phosphoric acid as mobile phase with gradient elution. The flow rate was 1.0 mL·min^-1. The detection wavelength was set at 330 nm. Results:The calibration curves were linear within the range of 0.049 92-0.898 6 μg for rosmarinic acid,0.677 6-3.388 0 μg for baicalin and 0.083 50-0.453 6 μg for baicalein. All ingredients showed a good linear relationship(r=0.999 9). The average recoveries ranged from 100.3%-102.6% with RSDs below 1.3%. And the contents in 15 batches of samples were 0.02-0.15,3.71-7.59 and 0.16-1.25 mg per tablet. Conclusion:The method is proved to be accurate. It provides a more comprehensive scientific basis for the quality evaluation of Duzhong Jiangya tablets.

关 键 词：杜仲降压片 迷迭香酸 黄芩苷 黄芩素 质量标准 薄层色谱法 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]