明目上清丸质量标准改进  

Improvement of the quality control standard for Mingmu Shangqing pills

作　　者：陆静娴 谭春梅 陈碧莲 马临科 祝明 

机构地区：[1]浙江省食品药品检验研究院,杭州310000

出　　处：《药物分析杂志》2016年第11期2051-2058,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:对明目上清丸(大黄、黄连、栀子、赤芍、当归和黄芩)的质量标准进行改进。方法:采用TLC法鉴别处方中的栀子、赤芍、当归、黄芩和黄连;采用HPLC法,以甲醇-0.2%磷酸水溶液为流动相,梯度洗脱的方法测定大黄中大黄酸、大黄素、大黄酚和大黄素甲醚,以乙腈-0.04 mol·L^(-1)磷酸二氢钾溶液为流动相,测定黄连中巴马汀和小檗碱。结果:薄层色谱中特征性斑点明显,分离度好,阴性对照无干扰;大黄酸、大黄素、大黄酚和大黄素甲醚分别在6.5~162.8 ng(r=1.000 0)、12.4~311.0 ng(r=1.000 0)、13.8~345.4 ng(r=1.000 0)、3.2~80.8 ng(r=0.999 8)范围内与峰面积均呈良好的线性关系;平均回收率(n=9)分别为97.0%、98.0%、100.2%和101.4%,RSD分别为1.2%、1.2%、1.4%和1.5%;盐酸巴马汀和盐酸小檗碱分别在13.1~326.4 ng(r=0.999 9)和42.8~1 070.0 ng(r=0.999 9)范围内与峰面积均呈良好的线性关系,平均回收率(n=9)分别为101.9%和97.6%。样品中大黄酸、大黄素及大黄酚的含量测定总和为0.23~0.84 mg·g^(-1),大黄酸、巴马汀和小檗碱(以盐酸巴马汀和盐酸小檗碱计)的含量测定结果分别为0.027~0.259、0.591~0.896和2.57~3.90 mg·g^(-1)。结论:鉴别方法专属性强、灵敏度高;定量方法简便快速,结果准确且重复性好。经方法学验证,本法可作为明目上清丸的质量控制方法。Objective： To improve the quality control standard for Mingmu Shangqing pills （ Rhei Radix et Rhizoma, Coptidis Rhizoma, Gardeniae Fructus, Paeoniae Radix Rubra, Angelicae Sinensis Radix and Scutellariae Radix ）. Methods： Gardeniae Fructus, Paeoniae Radix Rubra, Angelicae Sinensis Radix and Scutellariae Radix were identified by TLC. A gradient HPLC method using mobile phases containing methanol and 0.2% phosphoric acid was developed to determine the contents of rhein, emodin, chrysophanol and physcion in Rhei Radix et Rhizoma. An isocratic HPLC method with the mobile phase consisting of acetonitrile and 0.04 mol . L-1 potassium dihydrogen phosphate was adopted to determine the contents of palmatine and berberinein Coptidis Rhizoma. Results： Characteristic spots could be detected by TLC and well separated without the interference of negative samples. The calibration curves were linear in the ranges of 6.5-162.8 ng for rhein （ r=1.000 0 ）, 12.4-311.0 ng for emodin （ r=1.000 0 ）, 13.8-345.4 ng for chrysophanol （ r=1.000 0 ）, 3.2-80.8 ng for physcion （ r=0.999 8 ）. The average recoveries （ n=9 ） were 97.0%, 98.0%, 100.2% and 101.4%. RSDs were 1.2%, 1.2%, 1.4% and 1.5%, respectively. The calibration curves were linear in the ranges of 13.1-326.4 ng for palmatine hydrochloride （ r=0.999 9 ）, and 42.8-1 070.0 ng for berberine hydrochloride （ r=0.999 9 ）. The average recoveries （ n=9 ） were 101.9% and 97.6%, respectively. The content of the sum of rhein, emodin and chrysophanol in different batches ranged from 0.23 to 0.84 mg.g-1. The content of rhein, palmatine hydrochloride and berberine hydrochloride in different batches ranged from 0.027 to 0.259, 0.591 to 0.896 and 2.57 to 3.90 mg. g-1, respectively. Conclusion： The identification method is selective and sensitive, and the quantitative method is simple, rapid, accurate and repeatable. The established method is confirmed by methodology validation that it can be applied to the quality control of Mingmu Shangqing pills.

关 键 词：明目上清丸 大黄 黄连 栀子 赤芍 当归 黄芩 大黄酸 大黄素 大黄酚 大黄素甲醚 巴马汀 小檗碱 质量标准 薄层色谱 液相色谱 

分 类 号：R917[医药卫生—药物分析学]