UPLC-QqQ/MS法检测阿胶强骨口服液阿胶及杂皮源成分  

UPLC-QqQ-MS/MS Analysis of Donkey-hide Gelatin and Different Animal Skin Gelatin in Ejiao Qianggu Oral Liquid

作　　者：陈伟 范文玺[1] 王晓敏 马芹 CHEN Wei;FAN Wenxi;WANG Xiaomin;MA Qin(Xinjiang Hua Shidan Pharmaceutical Reaearch CO.LT,Urumqi 830011,China;Key Laboratory of Bone Health Traditional Chinese Medicine Research and Development in Xinjiang Production and Construction Corps,Urumqi 830011,China)

机构地区：[1]新疆华世丹药物研究有限责任公司,新疆乌鲁木齐830011 [2]新疆生产建设兵团骨健康中药研发重点实验室,新疆乌鲁木齐830011

出　　处：《中国民族民间医药》2023年第24期28-32,共5页Chinese Journal of Ethnomedicine and Ethnopharmacy

基　　金：十四五重大科技专项“阿胶强骨口服液”等特色大品种培育及中药民族药新药创制研究(2022A03107-2);第二师铁门关市中青年科技创新领军人才(2020RCTD03)。

摘　　要：目的:建立阿胶强骨口服液中阿胶及掺杂皮源成分的专属性检测方法。方法:用序列分析用胰蛋白酶对阿胶强骨口服液及掺入不同杂皮胶的伪品中胶类成分进行酶解,采用超高效液相色谱-三重四极杆质谱(UPLC-QqQ/MS),选择阿胶特征分子离子峰m/z 539.8→612.4及牛皮源特征肽A特征离子对m/z 641.3→726.2作为检测离子对,离子化模式为ESI+,进行多反应监测。同时,建立阿胶强骨口服液中马皮胶成分红外谱检测法,结合质谱法鉴别掺伪马皮胶样品。结果:3批购买的阿胶强骨口服液保留时间均与阿胶对照药材一致,在7.7 min出峰,未出现与牛皮胶溶液对应的牛皮特征色谱峰。6批掺入不同杂皮胶(牛皮胶、猪皮胶和马皮胶)中2批马皮胶自制口服液检测出阿胶对照特征峰;2批牛皮胶口服液样品检测出牛皮源特征峰。红外光谱结果显示马皮胶自制口服液在1400~1700 cm^(-1)处吸收峰较特异,可与其它胶质进行区别,补充阿胶强骨口服液对马皮源成分的鉴别。结论:该检测方法专属性强,可用于阿胶强骨口服液中阿胶及杂皮源成分的检测,为阿胶强骨口服液质量标准提升提供了新的思路和方法。Objective To establish an exclusive analytical method to identify donkey-hide gelatin and other source gelatin in Ejiao Qianggu Oral Liquid.Methods Identification of donkey-hide gelatin and others source gelatin in Ejiao Qianggu Oral Liquid was performed by the Multiple Reaction Monitoring of rapid resolution liquid chromatography(UPLC)coupled to triple quadruple mass spectrometry(QqQ),and quantitative ion pair of 539.8→612.4(m/z,Da),641.3→762.2(m/z,Da)were respective used for the detection of the cow skin origin and Ejiao control ingredients.Further,the horse hide glue and donkey-hide gelatin was distinguished by FT-IR.Results Characteristic molecular peaks of donkey-hide gelatin were detected in the three batches of commercially available Ejiao Qianggu Oral Liquid samples,of which three batches of cowhide source were not detected.Meanwhile,two batches of characteristic peaks of horse-hide gelatin were detected in six batches of homemade oral liquid samples and two batch contained elements of cowhide source,either component of donkey-hide gelatin was not detected in the six batches.It must be added,the IR absorption peaks in 400~1700 cm^(-1)of horse hide glue was more specific than others gelatin,that compensate for the identification of horse-hide gelatin.Conclusion Methodological verification shows that the established method is specific,and suitable for the identification of donkey-hide gelatin and others source in Ejiao Qianggu Oral Liquid.This research has provided theoretical support for the optimizing of Ejiao identification methods,and quality evaluation.

关 键 词：阿胶强骨口服液 超高效液相色谱-三重四级杆质谱 红外光谱 阿胶 

分 类 号：R284.1[医药卫生—中药学]