摘要
目的:研究复方木尼孜其颗粒(CMG)的质量控制方法,为制定其质量标准提供参考。方法:分别以甘草苷、异甘草苷、甘草酸、骆驼蓬碱、去氢骆驼蓬碱和异株五加甲苷为定性、定量指标,建立CMG中甘草、骆驼蓬子、黑种草子3种药材的薄层鉴别及含量测定方法。以硅胶HSGF254为薄层色谱板,正丁醇-水-甲醇-三乙胺为展开剂,10%硫酸乙醇试剂显色后分别在日光和紫外366 nm条件下检视,进行TLC定性分析。采用C18色谱柱,以乙腈-乙酸铵为流动相,ELSD为检测器,建立HPLC定量分析方法。模拟口服给药胃肠道生理条件,以酸水处理制剂,建立指纹图谱,指认共有峰,为制剂到体内后的整体特征提供信息。结果:在建立的TLC条件下,可在紫外366 nm条件下检视去氢骆驼蓬碱和骆驼蓬碱,在日光下检视甘草苷和异株五加甲苷。甘草苷、异甘草苷、甘草酸、骆驼蓬碱、去氢骆驼蓬碱和异株五加甲苷质量浓度分别在14.66~469.20、3.11~99.40、12.51~400.40、22.13~708.00、18.93~605.60和12.58~402.40μg·mL^(-1)范围内呈良好线性关系,方法平均回收率及RSD分别在99.4%~101.1%和1.8%~3.0%范围内;10批样品中上述6个成分的平均含量分别为(1.37±0.23)、(0.30±0.04)、(1.72±0.23)、(4.16±0.55)、(2.27±0.36)和(2.21±0.40)mg·袋-1。CMG经酸水处理后供试液指纹图谱中18个共有峰保留时间的RSD均<0.5%,峰面积的RSD均<3.0%,除上述已指认的4个指标成分外还鉴定出4个成分:绿原酸,咖啡酸,阿魏酸,芹菜素-7-O-葡萄糖苷。结论:建立的定性及定量方法适用于CMG中多个活性成分的质量控制。
Objective：To study the quality control methods and to provide reference for establishing quality criteria of compound Muniziqi granules（CMG）. Methods：Using liquiritin,isoliquiritin,glycyrrhizic acid,harmaline,harmine,and sieboldianoside A as the qualitative and quantitative markers,TLC and HPLC methods were established for identification and assay of Glycyrrhizae Radix et Rhizoma,Pegani Semen and Nigellae Semen in CMG. The TLC method was developed by using 1-butanol-water-methanol-triethylaminemixture as developing solvent on HSGF254. The thin-layer plate was inspected under the condition of sunlight and UV 366 nm respectively after coloration with 10% sulfuric acid ethanol. The HPLC method was performed on a C18 column and the mobile phase was consisted of acetonitrile-ammonium acetate with gradient elution. Evaporative light scattering detector（ELSD） was used as detector. In order to provide overall in vivo features of CMG,HPLC fingerprint of CMG treated with acid solution（simulating gastrointestinal physiological condition） was set up and common peaks were identified. Results：Under the condition of the established TLC method,harmaline and harmine could be identified under UV 366 nm,liquiritinand and sieboldianoside A could be identified under sunlight. Liquiritin,isoliquiritin,glycyrrhizic acid,harmaline,harmine,and sieboldianoside A showed ideal linearity within the ranges of 14.66-469.20 μg·mL^（-1）,3.11-99.40 μg·mL^（-1）,12.51-400.40 μg·mL^（-1）,22.13-708.00 μg·mL^（-1）,18.93-605.60 μg·mL^（-1） and 12.58-402.40 μg·mL^（-1）,respectively. The average recovery and RSD were between 99.42%-101.06% and 1.8%-3.0% respectively. The average contents of liquiritin,isoliquiritin,glycyrrhizic acid,harmaline,harmine,and sieboldianoside A in 10 batches of CMG were（1.37±0.23）,（0.30±0.04）,（1.72±0.23）,（4.16±0.55）,（2.27±0.36）,and（2.21±0.40） mg per bag,respectively. The RSD values of the relative retention time and area of 18 common peaks in HPLC fi
作者
韦悦
程娟娟
程雪梅
穆丹丹
王峥涛
王长虹
WEI Yue CHENG Juan-juan CHENG Xue-mei MU Dan-dan WANG Zheng-tao WANG Chang-hong(Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, The MOE Key Laboratory for Standardization of Chinese Medicines and Shanghai Key Laboratory of Compound Chinese Medicine,Shanghai R＆D Centre for Standardization of Chinese Medicine, Shanghai 201203, China Xinjiang Uygur Pharmaceutical Co. Ltd., Urumqi 830000, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第10期1799-1809,共11页
Chinese Journal of Pharmaceutical Analysis
基金
上海市国内科技合作领域项目(14495800200)
新疆维吾尔自治区科技支疆计划项目(2013911134)
关键词
复方木尼孜其颗粒
维吾尔药
甘草
骆驼蓬子
黑种草子
甘草苷
异甘草苷
甘草酸
骆驼蓬碱
去氢骆驼蓬碱
异株五加甲苷
中药质量控制
compound Muniziqi granules
uyghur medicine
Glycyrrhizae Radix et Rhizoma
Pegani Semen
Nigellae Semen
liquiritin
isoliquiritin
glycyrrhizic acid
harmaline
harmine
sieboldianoside A
qualitycontrol of Traditional Chinese medicine
