超高效液相色谱串联三重四极杆质谱法检查脑立清制剂中水麦冬酸成分  

Test of triglochinic acid in Naoliqing preparations by ultra high performance liquid chromatography-triple quadrupole mass spectrometry

作　　者：于凤蕊 钱利民 尹雪 焦阳 徐兴燕 林永强 YU Fengrui;QIAN Limin;YIN Xue;JIAO Yang;XU Xingyan;LIN Yongqiang(NMPA Key Laboratory for Quality Evaluation of Gelatin Products,Shandong Engineering Laboratory for Standard Innovation and Quality Evaluation of TCM,Shandong Institute for Food and Drug Control,Jinan 250101,China;The First Affiliated Hospital of Shandong First Medical University,Jinan 250014,China)

机构地区：[1]山东省食品药品检验研究院,国家药品监督管理局胶类产品质量评价重点实验室,山东省中药标准创新与质量评价工程实验室,山东济南250101 [2]山东第一医科大学第一附属医院,山东济南250014

出　　处：《药学研究》2023年第2期113-116,共4页Journal of Pharmaceutical Research

基　　金：山东省人文社会科学课题(No.2021-YYGL-44);山东省重点研发计划(No.2021CXGC010511)。

摘　　要：目的建立脑立清制剂中水麦冬酸成分的检测方法。方法样品经萃取富集后,利用超高效液相色谱-三重四极杆质谱(UPLC-MS/MS),以水麦冬酸为指标成分,对脑立清制剂中常见掺伪虎掌南星情况进行监控。采用Waters ACQUITY UPLC HSS T3 C 18(2.1 mm×100 mm,1.8μm)色谱柱,以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,体积流量0.2 mL·min^(-1);柱温30℃,进样量2μL;质谱条件采用ESI-多反应监测(MRM)模式扫描,选择m/z 187.0→143.3和m/z 187.0→98.9作为检测离子对。结果以所建立的方法对88批次脑立清制剂进行检测,结果5个厂家的15批样品检查出水麦冬酸成分。结论所建立的方法准确可靠,专属性强,可用于脑立清制剂中的水麦冬酸成分的检查;同时也为其他含半夏制剂中掺伪虎掌南星的监控提供参考。Objective To establish an analysis method for the determination of triglochinic acid in Naoliqing preparations.Methods After extracted and enriched,the samples were analyzed using ultra high performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS),and the adulterant of Pinelliae Pedatisectae Rhizoma in Naoliqing preparations was monitored by using triglochinic acid as index component.The samples were separated by Waters ACQUITY UPLC HSS T3 C 18 column(2.1 mm×100 mm,1.8μm),eluted by gradient with acetonitrile-0.1%formic acid solution as mobile phase,with flow rate of 0.2 mL·min^(-1);Column temperature of 30℃,injection volume of 2μL;Electrospray ionization source was used negative ion mode and multiple reaction monitoring(MRM)mode was performed with transitions of m/z 187.0→143.3 and m/z 187.0→98.9.Results 88 batches of Naoliqing preparations were detected by the established method,triglochinic acid were found in 15 batches of samples from 5 manufactures.Conclusion The proposed method method was specific,precise,reliable,and suitable for identification of triglochinic acid in Naoliqing preparations;At the same time,it also provides a reference for the monitoring of Pinelliae Rhizoma adulterated with Pinelliae Pedatisectae Rhizoma in preparations.

关 键 词：脑立清制剂 清半夏 虎掌南星 水麦冬酸 超高效液相色谱-三重四极杆质谱 

分 类 号：R284.1[医药卫生—中药学]