参松养心胶囊多组分同时测定及方法学验证  

Simultaneous determination of different constituents in Shensong Yangxin capsules and method validation

作　　者：白一丹 乔洲 薛敬伟[2] 刘富垒[2] 柳文媛[1] BAI Yi-dan;QIAO Zhou;XUE Jing-wei;LIU Fu-lei;LIU Wen-yuan(Key Laboratory of Drug Quality Control and Pharmacovigilance（China Pharmaceutical University）,Ministry of Education,Nanjing 210009,China;Shandong Taian Central Hospital,Taian 271000,China)

机构地区：[1]药物质量与安全预警教育部重点实验室(中国药科大学),南京210009 [2]山东省泰安市中心医院,泰安271000

出　　处：《药物分析杂志》2018年第8期1358-1368,共11页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立高效液相色谱法同时测定参松养心胶囊中8个主要成分莫诺苷、马钱苷、芍药苷、丹酚酸B、五味子酯甲、丹参酮Ⅰ、五味子甲素和丹参酮Ⅱ_A的含量并对方法学进行验证。方法:以L_9(3~4)正交试验优化提取条件,采用50%甲醇超声提取75 min,料液比为0.4 g∶10 mL。液相色谱分析采用ODS-2 C_(18)色谱柱(4.6 mm×250 mm,5μm),柱温30℃,以甲醇-乙腈(1∶1)及甲酸溶液(pH3)为流动相,梯度洗脱,流速1.1 mL·min^(-1),检测波长230 nm。结果:莫诺苷、马钱苷、芍药苷、丹酚酸B、五味子酯甲、丹参酮Ⅰ、五味子甲素和丹参酮Ⅱ_A分别在19.84～198.40μg·mL^(-1)(r=0.999 0)、10.20～101.98μg·mL^(-1)(r=0.999 3)、26.76～267.62μg·mL^(-1)(r=0.999 4)、94.32～943.24μg·mL^(-1)(r=0.999 6)、4.50～45.01μg·mL^(-1)(r=0.999 5)、4.95～49.45μg·mL^(-1)(r=0.999 9)、3.11～31.12μg·mL^(-1)(r=0.999 5)和2.96～29.61μg·mL^(-1)(r=0.999 5)范围内呈良好线性关系,平均加样回收率在100.3%～109.1%之间。10批样品中上述8个成分的含量范围分别为1.548～2.113、1.455～1.641、2.523～3.706、5.535～13.255、0.654～0.866、0.168～0.429、0.329～0.496和0.216～0.407 mg·g^(-1)。结论:本研究建立的方法可以用于中成药参松养心胶囊的多组分同时测定。Objective：To establish a method for simultaneous determination of eight constituents in Shensong Yangxin capsules and validate the method.Methods：The L9（3～4）orthogonal design was carried out in order to optimize the extraction method.The method of extraction was 50% methanol,the ratio of sample and solvent was 0.4 g∶10 mL and 75 min for ultrasonication.The HPLC analysis was performed on an ODS-2 C_（18） column（4.6 mm×250 mm,5 μm）at 30 ℃,with 0.4% formic acid and methanol-acetonitrile（1∶1）as the mobile phase by gradient elution at a flow rate of 1.1 m L·min-1.The detection wavelength was 230 nm.Results：Good linearities of morroniside,loganin,paeoniflorin,salvia acid B,schisantherin A,tanshinone Ⅰ,schisandrin A and tanshinone ⅡA were achieved in the range of 19.84-198.40 μg·mL-1（r=0.999 0）,10.20-101.98 μg·mL-1（r=0.999 3）,26.76-267.62 μg·mL-1（r=0.999 4）,94.32-943.24 μg·mL-1（r=0.999 6）,4.50-45.01 μg·mL-1（r=0.999 5）,4.95-49.45 μg·mL-1（r=0.999 9）,3.11-31.12 μg·mL-1（r=0.999 5）and 2.96-29.61 μg·mL-1（r=0.999 5）,respectively.The average recoveries were between 100.3% and 109.1%.The concent ranges of morroniside,loganin,paeoniflorin,salviaacid B,schisantherin A,tanshinone Ⅰ,schisandrin A and tanshinone ⅡA in 10 batches of samples were 1.548-2.113 mg·g-1,1.455-1.641 mg·g-1,2.523-3.706 mg·g-1,5.535-13.255 mg·g-1,0.654-0.866 mg·g-1,0.168-0.429 mg·g-1,0.329-0.496 mg·g-1 and 0.216-0.407 mg·g-1,respectively. Conclusion：The method can be used to quantify multi-constituents simultaneously in Shensong Yangxin capsules.

关 键 词：参松养心胶囊 多组分测定 莫诺苷 马钱苷 芍药苷 丹酚酸B 五味子酯甲 丹参酮 五味子甲素 正交试验 高效液相色谱法 方法学验证 

分 类 号：R917[医药卫生—药物分析学]