川楝子水提化学成分的UPLC-ESI-Q-TOF-MS分析  

Chemical constituents from water extract of Toosendan Fructus by UPLC-ESI-Q-TOF-MS

作　　者：李振华[1,2] 徐金娣[1] 鞠建明[1] 朱亚楠[1,2] 王璐璐[1] 

机构地区：[1]江苏省中医药研究院中药分析与代谢组研究室,江苏南京210028 [2]南京中医药大学药学院,江苏南京210046

出　　处：《中草药》2015年第4期496-501,共6页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金项目(81102467);天然药物活性组分与药效国家重点实验室开放课题(SKLNMKF201208-1)

摘　　要：目的通过UPLC-ESI-Q-TOF-MS技术定性分析川楝子水提取物中的主要化学成分。方法采用ACQUITY HSS T3色谱柱(100 mm×2.1 mm,1.8μm),并以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,体积流量为0.4 m L/min,质谱使用ESI离子源,正负离子模式扫描采集数据。结果通过正负离子质谱信息及元素组成分析,并结合相关文献和对照品数据对照,鉴定出了川楝子水提取物中的15个化合物,分别为香草酸、丁香酸、对羟基苯甲酸、芦丁、meliatoosenin E、川楝素、Δ5,6-异川楝素、异川楝素、meliatoosenin N、meliatoosenin P、1-deacetylnimbolinin B、meliatoosenin R、1-O-tigloyl-1-O-debenzoylohchinal、meliatoosenin R及nimbolinin B。结论利用UPLC的高效分离能力和MS的高灵敏度检测优势,建立了一种基于UPLC-ESI-Q-TOF-MS的定性分析方法,为控制川楝子药材饮片的质量、稳定其临床疗效及阐释其作用机制提供了科学依据。Objective To analyze and identify the chemical constituents from the water extract of Toosendan Fructus by UPLC-ESIQ-TOF-MS. The analysis was performed on an ACQUITY HSS T3 reverse phase column（2.1 mm × 100 mm, 1.8 μm）. The mobile phase consisted of acetonitrile and 0.1% formic acid was used for gradient elution, the flow rate was 0.4 m L/min. Methods Quadrupole-time of flight-mass spectrometry was applied for the qualitative analysis under positive and negative ion modes and ESI ion source was used for mass spectra. Results The results indicated that fifteen compounds from the water extract of Toosendan Fructus had been identified by direct comparison in both positive and negative ion mass data, the element compositions analysis, and the data of the literature. They are vanillic acid, lilac acid, p-hydroxybenzoic acid, rutin, meliatoosenin E, toosendanin, Δ5,6-isotoosendanin, isotoosendanin, meliatoosenin N, meliatoosenin P, 1-deacetylnimbolinin B, meliatoosenin R, 1-O-tigloyl-1-O-debenzoylohchinal, meliatoosenin R, and nimbolinin B. Conclusion The efficient separation ability of UPLC and high sensitive detection of MS are used in this study, which will provide the evidences for evaluating the quality of Toosendan Fructus herbs, stabilizing the curative effect in clinic, and explaining the mechanism.

关 键 词：川楝子 UPLC-ESI-Q-TOF-MS 川楝素 香草酸 丁香酸 

分 类 号：R284.1[医药卫生—中药学]