HPLC-QTOF-MS法鉴别雷公藤多苷工艺残渣中的化学成分  

Identification of major constituents from process residue of tripterygium glycosides by HPLC-QTOF-MS

作　　者：李明炀 侯继芹 韦丹丹[1] 江振洲[2] 严明[2] 汪豪[1] 

机构地区：[1]中国药科大学天然药物化学教研室天然药物活性组分与药效国家重点实验室,南京210009 [2]中国药科大学新药筛选中心,南京210009

出　　处：《中国药科大学学报》2015年第6期689-695,共7页Journal of China Pharmaceutical University

基　　金：国家自然科学基金资助项目(No.81172955);江苏高校青蓝工程中青年学术带头人资助项目~~

摘　　要：建立高效液相色谱串联四级杆飞行时间质谱法(HPLC-QTOF-MS)快速鉴定雷公藤多苷柱色谱工艺残渣化学成分。采用Zorbax SB-C_(18)色谱柱(4.6mm×50 mm,1.8μm),流动相为乙腈-0.2%甲酸溶液,梯度洗脱,采用ESI-Q-TOF检测,正离子模式扫描。根据色谱峰精确相对分子质量、碎片离子信息及液相色谱保留时间比较鉴别化合物。结果表明,采用HPLC-QTOF-MS法鉴定了雷公藤多苷工艺残渣中30个成分,包括15个生物碱类化合物,10个二萜类化合物,4个三萜类化合物,1个不饱和脂肪酸。本研究工作为雷公藤多苷工艺残渣的综合开发利用提供定性分析依据。A qualitative analytical method of liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry （HPLC-QTOF-MS） was developed for identification of major constituents in process residue of tripterygium glycosides. The HPLC-QTOF-MS assay was performed on a Zorbax SB-Cls column （4. 6 mm × 50 mm, 1.8 μm） with the mobile phase consisting of acetonitrile and water containing 0. 2% formic acid in gradient mode. Positive ion mode was used for TOF-MS. According to the accurate molecular weight, MS fragment pathway, comparison with the retention time of reference compounds, total 30 compounds, including fifteen alkaloids, ten diterpenoids, four triterpenoids and an unsaturated fatty acid were identified or tentatively characterized in process residue of tripterygium glycosides. This study may be helpful to the comprehensive exploitation and utilization of process residue of tripterygium glycosides.

关 键 词：雷公藤多苷 工艺残渣 HPLC-QTOF-MS 定性分析 

分 类 号：R284.1[医药卫生—中药学] O657.63[医药卫生—中医学]