基于UHPLC-Q-TOF/MS技术快速分析消痰通腑方化学成分
投稿时间:2021-09-06  修订日期:2022-03-03  点此下载全文
引用本文:秦烨,黄玮,顾雨芳,张慈安,修丽娟,唐继贵,张凤,刘煊.基于UHPLC-Q-TOF/MS技术快速分析消痰通腑方化学成分[J].药学实践杂志,2022,40(4):339~346
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作者单位E-mail
秦烨 中国人民解放军中部战区总医院, 湖北 武汉 430014  
黄玮 上海市闵行区古美社区卫生服务中心, 上海 201102  
顾雨芳 海军军医大学长征医院, 上海 200003  
张慈安 海军军医大学长征医院, 上海 200003  
修丽娟 海军军医大学长征医院, 上海 200003  
唐继贵 海军军医大学长征医院, 上海 200003  
张凤 海军军医大学长征医院, 上海 200003 fengzhangky@aliyun.com 
刘煊 海军军医大学长征医院, 上海 200003 18616630816@163.com 
基金项目:国家自然科学基金资助项目(No.81804008)
中文摘要:目的 探明消痰通腑方的主要化学成分,为方剂药效物质基础研究和临床治疗提供科学依据。方法 采用超高效液相色谱四极杆飞行时间质谱法(UHPLC-Q-TOF/MS)对消痰通腑方化学成分进行鉴定,色谱条件为Waters ACQUITY UPLC BEH C18色谱柱(2.1mm×100 mm,1.7 μm),以 0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,柱温30 ℃,流速0.3 ml/min,进样量1 μl,检测波长254 nm;质谱条件为电喷雾离子源(ESI),正、负离子全扫描模式采集质谱数据,根据对照品、自建质谱数据库和在线获得的化合物质谱数据库对色谱峰进行物质鉴定。结果 初步鉴定出55个化合物,分别来自黄连、重楼、大黄、天南星、法半夏。结论 本文所建立的UHPLC-Q-TOF/MS方法能系统、准确地鉴别消痰通腑方的化学成分,可为该方剂的质量标志物筛选和有效成分研究提供参考。
中文关键词:超高效液相色谱串联四极杆飞行时间质谱  化学成分  消痰通腑方
 
Rapid analysis of chemical components of Xiaotan Tongfu formula based on UHPLC-Q-TOF/MS
Abstract:Objective To rapidly explore the chemical components of Xiaotan Tongfu formula, and to provide scientific basis for the basic research and clinical treatment of the formula. Methods Analysis was performed on an Agilent 1290 ultra-performance liquid chromatography system coupled with an Agilent 6530 accurate quality Q-TOF/MS system, by using a Waters ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm), with a gradient elution applying 0.1% aqueous formic acid solution and acetonitrile as a mobile phase. The flow rate was 0.3 ml/min. The column temperature was 30℃. The injection volume was 1 μl, and the detection wavelength was 254 nm. Mass spectrometry (MS) data were collected in both positive and negative ESI ion modes. Components in the formula were identified by using the in-house compound database, and comparing the retention time (tR), MS1 and MS2 data with the standard compounds, and the online compound MS database. Results A total of 55 compounds were identified from Coptis coptidis, Pseudomonas solani, Rhubarb, Araceae artemisiae and Pinellia chinensis. Conclusion The established UHPLC-Q-TOF/MS method could systematically and accurately identify the chemical components from Xiaotan Tongfu formula, and provided a reference for the quality marker selection and the research on the active ingredient.
keywords:UHPLC-Q-TOF/MS  chemical components  Xiaotan Tongfu formula
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