排石颗粒高效液相色谱法指纹图谱研究及薄层色谱鉴别  

Research on HPLC Fingerprint and TLC Identification of Paishi Granules

作　　者：李柯城 袁铭铭 熊晓丽 周国平 LI Kecheng;YUAN Mingming;XIONG Xiaoli;ZHOU Guoping(Jiangxi University of Traditional Chinese Medicine,Nanchang Jiangxi 330004,China;Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang Jiangxi 330029,China.)

机构地区：[1]江西中医药大学,江西南昌330004 [2]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,江西南昌330029

出　　处：《药品评价》2021年第22期1364-1368,共5页Drug Evaluation

基　　金：江西省重点研发计划项目(20171BBG70104)。

摘　　要：目的:建立排石颗粒高效液相色谱法(HPLC)指纹图谱分析方法,及排石颗粒薄层色谱(TLC)鉴别。方法:HPLC法:Thermo Scientific C18(4.6 mm×250 mm,5 μm)色谱柱,以乙腈∶甲醇(1∶1)(A)-0.05%磷酸水溶液(B)为流动相进行梯度洗脱,体积流量1.0 mL/min;检测波长284 nm。并结合中药色谱指纹图谱相似度评价软件(2004A版)进行相似度分析。TLC法:HPTLC Silica gel 60 薄层板,展开剂为三氯甲烷-甲醇-水(15∶9∶1),显色剂为10%硫酸乙醇。结果:建立了15个批次排石颗粒HPLC指纹图谱,确定了25个共有峰,归属了12个未知峰,指认了5个主要色谱峰,15批样品指纹图谱相似度均大于0.95。TLC中akemisaponin E、皂苷 PJ1分离效果较好。结论:该研究建立的方法重复性好,耐用性高,可用于排石颗粒质量控制。Objective:To establish HPLC fingerprint analysis method and TLC identification method for paishi granules.Methods:HPLC method:The chromatographic column of Thermo Scientific C18 (4.6 mm×250 mm,5 μm) was used for gradient elution with acetonitrile:methanol (1∶1) (A)-0.05% phosphoric acid aqueous solution (B) as mobile phase at a volume flow rate of 1.0 mL/min.The detection wavelength was 284 nm.The similarity analysis of 15 batches of paishi granules was carried out in combination with the similarity evaluation software of traditional Chinese medicine chromatographic fingerprint (2004A version).TLC method:HPTLC Silica gel 60 thin laminate was prepared with chloroform methanol-water (15∶9∶1) as developing agent and 10% sulfuric acid ethanol as chromogenic agent.Results:HPLC fingerprint of paishi granules was established,25 common peaks were identified,12 unknown peaks were assigned,and 5 major peaks were identified.The similarity of fingerprint of 15 batches of samples were all greater than 0.95.The separation effect of akemisaponin E and saponin PJ1 in TLC was better.Conclusion:The method established in this study has good repeatability,high durability,and can be used for the quality control of paishi granules.

关 键 词：排石颗粒 指纹图谱 木通 高效液相色谱法 薄层色谱 

分 类 号：R284.1[医药卫生—中药学]