摘要
目的：改进保肾片的质量控制标准,为制剂生产提供质量保障.方法：采用TLC法对制剂中的大黄进行定性鉴别;采用HPLC法对制剂中的大黄酸、大黄素、大黄酚总含量进行测定,其色谱条件为：色谱柱为Lichrospher-C18柱（250 mm×4.6mm,5μm）,流动相为甲醇-0.1％磷酸溶液（70：30）,流速为1.0 ml·min-1,柱温为30℃,检测波长为254 nm.结果：TLC鉴别色谱斑点清晰,阴性无干扰;大黄酸在0.001 3～0.0106 mg·ml-1范围内有良好的线性关系（r =0.999 9）,大黄素在0.002 7 ～0.021 3 mg·ml-1范围内有良好的线性关系（r =0.999 9）,大黄酚在0.007 6 ～0.060 5 mg· ml.1范围内有良好的线性关系（r =0.999 9）,平均回收率分别为100.18％、100.31％、100.09％,RSD分别为1.08％、0.67％、1.11％（n=9）.结论：该方法准确易行,便于质量控制.
Objective： To improve the determination method for the total anthraquinone in Baoshen tablets to control the quality. Methods： TLC was used for the qualitative identification of Rheum officinale Baill.. HPLC was used to determine the content of total anthraquinone in the tablets. The determination was performed on a Lichrospher-Cl8 column（250 mm ×4.6 mm,5 μm）with the mobile phase of methanol-0.1% H3 PO4 （ 70：30 ）. Tile flow rate was 1.0 ml · min - 1, the column temperature was at 35 ℃ and the detection wavelength was 254nm. Results： The spots on the TLC plates were clear without negative interference. The linear range of rhein, emo- din and chrysophanol was obtained within 0. 001 3-0.010 6 mg· ml - l （ r = 0.999 9 ）, 0.002 7-0.021 3 mg · ml - 1 （ r = 0.999 9 ） and 0.007 6-0.060 5 mg · m1-1 （r =0.999 9）, the average recovery was 100.18%, 100.31% and 100.09% , and RSD was 1.08% , 0.67% and 1.11% （n = 9 ）, respectively. Conclusion： The improved method is accurate and feasible. It can be used very conven- iently in the quality control.
出处
《中国药师》
CAS
2014年第8期1300-1302,共3页
China Pharmacist
基金
全军医疗机构制剂标准提高科研专项课题重点项目(编号:13ZJZ13)
