痰热清注射液中熊胆粉提取物的UPLC指纹图谱研究  

Research on UPLC Fingerprint of Pulvis Fellis Ursi Extract in Tanreqing Injection

作　　者：苗水[1] 李雯婷[1] 刘绍勇 张小利 胡青[1] 毛秀红[1] 季申[1] Miao Shui;Li Wenting;Liu Shaoyong;Zhang Xiaoli;Hu Qing;Mao Xiuhong;Ji Shen(Shanghai Institute for Food and Drug Control,NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai 201203,China;Shanghai Kaibao Pharmaceutical Co.Ltd.)

机构地区：[1]上海市食品药品检验所,国家药品监督管理局中药质量控制重点实验室,上海201203 [2]上海凯宝药业股份有限公司

出　　处：《中国药师》2021年第6期1156-1160,共5页China Pharmacist

基　　金：科技部重点研发专项(编号:2017YFC1700800)。

摘　　要：目的:建立痰热清注射液中熊胆粉提取物的UPLC指纹图谱产品质量控制方法,缩短分析时间。方法:采用高分辨质谱技术对痰热清注射液(TRQI)中熊胆粉提取物的共有峰进行了归属,共鉴定出4个胆酸类成分。采用Waters ACQUITY UPLC BEH C_(18)色谱柱(0.3 cm×10 cm,1.7μm),以乙腈-0.1%磷酸为流动相,梯度洗脱,流速:0.6 ml·min^(-1),柱温:35℃,检测波长:203 nm,建立了痰热清注射液中熊胆粉提取物的UPLC指纹图谱分析方法。结果:采用"中药色谱指纹图谱相似度评价系统2.0版"对33批痰热清注射液指纹图谱进行评价分析,各批次痰热清注射液与对照指纹图谱间的相似度均大于0.99。结论:本方法首次建立了痰热清注射液中熊胆粉提取物的UPLC指纹图谱,分析时间小于10 min,大幅提升了质控效率。Objective:To establish a UPLC fingerprint method for Pulvis Fellis Ursi extract in Tanreqing injection(TRQI)to reduce the total analysis time.Methods:The common peaks of the extract of Pulvis Fellis Ursi in TRQI were identified by high resolution mass spectrometry.Four cholic acids were identified,which accounted for 93.2% of the total extract.A rapid UPLC fingerprint method for Pulvis Fellis Ursi extract in TRQI was established.The method was developed on a column of Waters ACQUITY UPLC BEH C18(0.3cm×10 cm,1.7μm)with acetonitrile-0.1% phosphoric acid solution as the mobile phase with gradient elution at a flow rate of 0.6 ml·min^(-1).The detection wavelength was 203 nm,and the column temperature was 35℃.Results:The similarity evaluation of 33 batches of TRQI was carried out according to the Similarity Evaluation System for Chromatographic Fingerprints of TCM.The similarity degrees of 33 batches of samples were all above 0.99.Conclusion:The UPLC fingerprint of Pulvis Fellis Ursi extract in TRQI is established for the first time.The analysis time is reduced from more than 90 minutes to shorter than 10 minutes,which greatly improves the quality control efficiency.

关 键 词：痰热清注射液 熊胆粉提取物 指纹图谱 超高效液相色谱 

分 类 号：R460.72[医药卫生—临床医学]