PDF《鄢长余,石亚囡,赵月然,高珊,姜范成,胡景莲 **,门启鸣 ...》

・624・ UPLC 法同时测定通脉颗粒中

5 个主成分的含量及其灰色关联度分析 * 鄢长余, 石亚囡, 赵月然, 高珊, 姜范成, 胡景莲 ** , 门启鸣 ** (大连市药品检验所, 大连 116021) 摘要 目的: 建立超高效液相色谱法同时测定通脉颗粒中丹参素、 原儿茶醛、 葛根素、 大豆苷和丹酚酸 B 含量, 并通过灰色关联度分析法对

5 种成分进行分析评价.

方法: 采用 XBridgeTM C18 色谱柱 (4.6 mm*75 mm, 2.5 μ m) , 以乙腈 (A) -0.2% 磷酸 (B) 为流动相, 梯度洗脱, 流速 0.7 mL・min-1 , 测定波长

280 nm.结果: 通脉颗粒中丹参素、 原儿茶醛、 葛根素、 大豆苷和丹酚酸 B 进样量分别在 0.011~0.106 μg (r=0.999 9) , 0.004~0.043 μg (r=0.999 9) , 0.019~0.193 μg (r=0.999 8) , 0.008~0.084 μg (r=0.999 9) , 0.005~0.048 μg (r=0.999 9) 范围内呈良好线性关系, 平均回收率 (n=9) 分别为 99.5%、 95.0%、 96.8%、 97.6%、 100.8%;

含量 测定结果分别在 0.18~18.

45、 0.01~0.

78、 0.04~9.

75、 0.01~1.

80、 0.05~1.58 mg・g-1 之间.通过灰色关联度方 法分析, 结果在 0.25~0.72 之间, 表明各生产企业之间产品质量差异较大.结论: 该方法为通脉颗粒的质量 控制和评价奠定了基础. 关键词: 通脉颗粒;

丹参;

川芎;

葛根;

丹参素;

原儿茶醛;

葛根素;

大豆苷;

丹酚酸 B;

含量测定;

灰色关联度;

超高效液相色谱 中图分类号: R

917 文献标识码: A 文章编号: 0254-1793 (2017) 04-0624-07 doi: 10.16155/j.0254-1793.2017.04.10 Simultaneous determination of

5 main components in Tongmai granules by UPLC and grey relational analysis * YAN Chang-yu, SHI Ya-nan, ZHAO Yue-ran, GAO Shan, JIANG Fan-cheng, HU Jing-lian** , MEN Qi-ming** (Dalian Institute for Drug Control, Dalian116021, China) Abstract Objective: To establish a UPLC method for simultaneous determination of danshensu, protocatechuic aldehyde, puerarin, daidzin and salvianolic acid B in Tongmai granules. To analyze and evaluate the

5 components with grey relational analysis. Methods: Separation was performed on a XBridgeTM C18 column (4.6 mm*75 mm, 2.5 μm) . And the mobile phase consisted of acetonitrile (A) and 0.2% phosphoric acid (B) with gradient elution at a flow rate of 0.7 mL・min-1 . The detection wavelength was

280 nm. Results: Danshensu, protocatechuic aldehyde, puerarin, daidzin and salvianolic acid B showed good linearity in the ranges of 0.011-0.106 μ g (r=0.999 9) , *

2015 年国家药品评价性抽验项目 ** 通信作者 胡景莲 Tel: (0411) 84255298;

E-mail:[email protected] 门启鸣 Tel: (0411) 84255200;

E-mail: [email protected] 第一作者 Tel: (0411) 84255298;

E-mail: [email protected] ・625・ 0.004-0.043 μg (r=0.999 9) , 0.019-0.193 μg (r=0.999 8) , 0.008-0.084 μg (r=0.999 9) , 0.005-0.048 μg (r=0.999 9) , respectively. The average recoveries (n=9) were 99.5%, 95.0%, 96.8%, 97.6%, 100.8%, respectively. Their contents in samples were between 0.18-18.45 mg・g-1 , 0.01-0.78 mg・g-1 , 0.04-9.75 mg・g-1 , 0.01-1.80 mg・g-1 , 0.05-1.58 mg・g-1 , respectively. Results of grey relational analysis were between 0.25 and 0.72, illustrating that the quality of the products from different manufacturing enterprises was greatly different. Conclusion: The method offered the foundation for the quality control and evaluation of Tongmai granules. Keywords: Tongmai granules;

Salviae Miltiorrhizae Radix et Rhizoma;

Chuanxiong Rhizoma;

Puerariae Lobatae Radix;

danshensu;

protocatechuic aldehyde;