消痔方醇提工艺和颗粒制剂含量测定方法  

Optimization on Alcohol Extraction Process of Xiaozhi Formulation and Determination of Emodin and Chrysophanol in Its Granules by HPLC

作　　者：李成职 刘洋[1] 刘小红[1] 高华[1] 孙世伟 侯玉雪 王威[1] 刘坤[1] LI Chengzhi;LIU Yang;LIU Xiaohong;GAO Hua;SUN Shiwei;HOU Yuxue;WANG Wei;LIU Kun(School of Pharmacy,Qingdao University,Qingdao 266021,China)

机构地区：[1]青岛大学药学院,山东青岛266021

出　　处：《青岛大学学报（工程技术版）》2018年第1期130-134,共5页Journal of Qingdao University(Engineering & Technology Edition)

基　　金：青岛市民生科技计划项目(15-9-2-88-nsh)

摘　　要：为了制备临床经验消痔方的口服颗粒制剂,本文以大黄素和大黄酚总量及出膏率为评价指标,建立消痔方中熟大黄和秦艽药材的醇提工艺。采用平行试验法对消痔方中熟大黄和秦艽药材的提取次数进行选择,采用正交试验优选乙醇体积分数、乙醇用量和提取时间,优化出最佳醇提工艺为加6倍量70%的乙醇,回流提取3次,提取时间为3h。颗粒制剂中大黄素和大黄酚的含量测定采用高效液相色谱法,色谱柱为Kramosil ODS(4.6 mm×250 mm,5μm),流动相为甲醇-0.1%磷酸溶液(80∶20),流速为1.0mL/min,检测波长为254nm,大黄素和大黄酚进样量分别在0.043 52~0.217 60μg和0.089 6~0.448 0μg范围内,峰面积积分值与进样量呈线性关系(r=0.999 9),平均加样回收率分别为98.35%和100.36%,相对标准偏差分别为2.07%和2.61%。该测定方法为消痔方口服固体医院制剂的研发提供了理论参考。To develop the hospital solid preparation of Xiaozhi formulation from veteran traditional Chinese medicine doctor,the alcohol extraction process of Rhei Radix et Rhizoma and Gentianae Macrophyllae Radix in Xiaozhi formulation was optimized.The content of emodin and chrysophanol and the dry paste rate were used as evaluation indexes.The number of extraction time was selected by single factor test.The optimum extraction condition was chosen by orthogonal design,including ethanol solution concentration,solvent to material ratio,and extraction period.The optimum extraction process was as follows:extracting three times with six times amount of 70%aqueous ethanol for 3 h.A high performance liquid chromatography method was established for the determination of emodin and chrysophanol in Xiaozhi formulation granules.The Kramosil ODS column was used as the stationary phase with themobile phase of methanol-0.1%phosphoric acid solution(80∶20).The detection wavelength was 254 nm.The linear ranges of emodin and chrysophanol were 0.043 52~0.217 60μg and 0.089 6~0.448 0μg with the correlation coefficient 0.999 9 between the injection quantity and the peak area.The average recoveries were 98.35%and 100.36%with the RSDs of 2.07%and 2.61%.The study will provide basis for the hospital preparation development of xiaozhi formulation granules.

关 键 词：消痔方颗粒 提取工艺 正交试验 高效液相色谱法 大黄素 大黄酚 

分 类 号：R284.2[医药卫生—中药学]