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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* |
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(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) |
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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: |
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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 |