摘要
目的:建立心安宁片中葛根、山楂、制何首乌的TLC定性鉴别法和大黄素的高效液相色谱含量测定法.方法:以葛根素为对照品,采用氯仿-甲醇(3:1)为展开剂,在UV365nm下检视;以齐墩果酸为对照品,采用氯仿-乙醚(1:0.8)为展开剂,30%硫酸溶液为显色剂;以大黄素、大黄素甲醚为对照品,采用石油醚(30～60℃)-醋酸乙酯-冰醋酸(9:2:0.1)为展开剂,在UV365nm下检视,分别对心安宁片中葛根、山楂、制何首乌进行薄层色谱法鉴别.采用Hypersil BDS C18柱(4.6mm×250mm,5μm),甲醇-水-磷酸(90:30:0.2)为流动相,检测波长为288nm,流速为1.0ml·min-1,柱温为35℃.结果:葛根素、齐墩果酸和大黄素、大黄素甲醚斑点清晰,阴性对照无干扰.HPLC定量分析中,大黄素的线性范围为1.132～11.320μg·ml-1,r=0.9999,平均回收率为99.5%,(RSD=1.5%,n=9).结论:该方法简便,快速,结果准确,重现性好.可用于该制剂的质量控制.
Objective：To develop the TLC indentification for Radix Puerariae and Fructus Crataegi and Radix polygoni Multiflori Preparata and the quantitative analysis of Emodin by HPLC in Xin＇an Ning Tablets. Methods ;Radix Puerariae and Fructus Crataegi and Radix Polygoni Multiflori Preparata were identified by TLC,respectively,using puerarin and oleanolic acid and emodin and physcion as chemical reference substances,and chloroform-methanol（3 ： 1 ）and chloroform-diethyl ether（1 ： 0.8）and petroleum ether-ethyl acetate-glacial acetic acid（9 ：2 ： 0.1）as mobile phases. Emodion contents were determined by HPLC using the BDS reversed-phase column of Hypersil C18（4.6mm × 250mm,5μm）,the mobile phase was a combination of methanol-water-phosphoric acid （90 ： 30 ： 0.2）at the flow rate of 1.0ml · min^-1,and the detection wavelength was 288nm, and column temperature at 35℃. Results ：The TLC chromatograms of puerarin and oleanolic acid and emodin and physcion were of clearness, good separation, and no interference. The emodin contents in Xin＇an Ning Tablets were determined by HPLC,in the linear range of 1. 132 to 11. 320μg · ml^-1 ,r= 9999,and the recovery of 99.5% （RSD= 1.5%）. Conclusion：The method is simple ,quick ,accurate ,reproducible and can be used for the quality control of emodion of Xin＇an Ning Tablets.
出处
《中国药品标准》
CAS
2005年第4期50-53,共4页
Drug Standards of China
