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HPLC-TOF/MS快速鉴别相思藤中的化学成分
付振贺1,黄玉凤1,黄超君1,谢从景1,吕磊1,杜红丽1,赵亮1,焦杨2*
0
(1. 海军军医大学(第二军医大学)东方肝胆外科医院药材科, 上海 200438;
2. 广西医科大学药学院药理教研室, 南宁 530021
*通信作者)
摘要:
目的 采用高效液相色谱-飞行时间质谱(HPLC-TOF/MS)分析技术对中药材相思藤的化学成分进行快速鉴别分析。方法 采用安捷伦"Formula-Database Generator"软件自建包括28个化合物的相思藤化学成分数据库,运用HPLC-TOF/MS技术采集相思藤提取物的总离子流色谱图,根据各化学成分的精确质荷比(m/z),通过自动比对的方法进行鉴别分析。色谱柱为安捷伦Zorbax Eclipse SB-C18(3.0 mm×100 mm,3.5 μm)液相色谱柱,流动相为0.1%甲酸水溶液-乙腈,采用梯度洗脱,流速为0.4 mL/min,柱温25℃,紫外检测波长254 nm,进样量10 μL;质谱采用电喷雾离子(ESI)源,正离子模式和负离子模式监测,质量数扫描范围为m/z 100~1 200。结果 共鉴别出相思藤中15种化学成分,其中正离子模式下10种、负离子模式下11种,正、负离子模式下均有响应6种。结论 建立了基于HPLC-TOF/MS的分析方法,可快速鉴别中药材相思藤中的化学成分,阐明了相思藤的化学物质基础,为相思藤的质量控制及药理机制研究奠定了基础。
关键词:  相思藤  高效液相色谱法  飞行时间质谱  化学成分
DOI:10.16781/j.0258-879x.2018.03.0329
投稿时间:2017-12-28修订日期:2018-03-06
基金项目:
Rapid identification of chemical constituents in Yine Abrus (Xiangsiteng) by HPLC-TOF/MS
FU Zhen-he1,HUANG Yu-feng1,HUANG Chao-jun1,XIE Cong-jing1,Lü Lei1,DU Hong-li1,ZHAO Liang1,JIAO Yang2*
(1. Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Navy Medical University(Second Military Medical University), Shanghai 200438, China;
2. Department of Pharmacology, School of Pharmacy, Guangxi Medical University, Nanning 530021, Guangxi, China
*Corresponding author)
Abstract:
Objective To rapidly identify the chemical constituents in a traditional Chinese medicine Yine Abrus (Xiangsiteng) by high-performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF/MS) analysis technique. Methods A formula database including 28 compounds of Xiangsiteng was developed by Agilent software "Formula-Database Generator". The total ion chromatograms of the Xiangsiteng extracts were obtained by HPLC-TOF/MS, and the chemical components were identified by automatic matching method according to the exact mass-to-charge ratio of each chemical component. The separation was performed on a Agilent Zorbax Eclipse SB-C18 column (3.0 mm×100 mm, 3.5 μm). The mobile phase composing of acetonitrile and 0.1% formic acid aqueous solution was used for gradient eluting. The flowing rate was 0.4 mL/min; the temperature of column was 25℃; the UV detection wavelength was 254 nm; and the sample selection was 10 μL. The electrospray ionization (ESI) source was applied for MS analysis under positive ion and negative ion modes, with the mass scan range being m/z 100-1 200. Results HPLC-TOF/MS identified a total of 15 chemical components from Xiangsiteng extracts, including 10 in positive ion mode and 11 in negative ion mode, and 6 both in both positive and negative ion modes. Conclusion A rapid and efficient method for identifying the chemical components of traditional Chinese medicine Xiangsiteng by HPLC-TOF/MS has been established, and the chemical components of Xiangsiteng has been clarified, which lays a foundation for the quality control and further pharmacological study of Xiangsiteng.
Key words:  Yine Abrus  high-performance liquid chromatography  time-of-flight mass spectrometer  chemical constituent