利用HPLC-IT-TOF-MS表征通关藤化学轮廓

Chemical profile characterization of Marsdenia tenacissima using HPLC-IT-TOF-MS

目的利用HPLC-IT-TOF-MS对通关藤的化学轮廓进行全面地解析。方法通关藤甲醇超声提取后,采用Waters AcquityUPLCHSST3色谱柱,乙腈-0.1%甲酸水溶液梯度洗脱;采用正、负离子自动多级质谱模式检测。利用多个孕甾烷类对照品推导该类化合物的质谱裂解规律。结果通过与对照品比对,准确归属了6个绿原酸类化合物和15个孕甾烷衍生物;通过相关文献数据结合质谱裂解规律推导,初步鉴定了100个孕甾烷类衍生物、4个黄酮类化合物和2个绿原酸类化合物。结论利用HPLC-IT-TOF-MS技术能快速、准确地对通关藤的化学轮廓进行全面解析,为通关藤及其制剂消癌平的质量标准及体内药效物质研究提供有效信息。

Objective To in depth analyze the chemical profile ofMarsdenia tenacissima using HPLC-IT-TOF-MS.Methods The pulverized materials were exacted with methanol in an ultrasonication manner and then separated on a Waters Acquity UPLC HSS T3 column (100mm×2.1mm,1.8μm,Milford,MA,USA)that was eluted in gradient with 0.1%formic acid-acetonitrile.The data was collected using automatically triggered tandem mass spectrometric mode in positive/negative-ionization polarities.The mass fragmentation patterns of polyoxypregnane derivatives were proposed using some authentic compounds.Results Six chlorogenic acid derivatives and 15polyoxypregnane derivatives were definitely assigned by referring to reference components,whereas the other signals,including 100polyoxypregnane derivatives,four flavonoids,and two chlorogenic'acid derivativeswere tentatively annotated via matching the acquired information with those achieved information and the proposed mass fragmentation rules.Conclusion The research efficiently and accurately analyzed the chemical profile of M.tenacissima using HPLC-IT-TOF-MS,which will provide meaningful information for the quality evaluation and the therapeutic mechanism investigation of M.tenacissima as .well as its preparation Xiao-Ai-Ping.