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目的:采用HPLC-MS-MS法,对桑叶总生物碱部位中的各生物碱成分进行分析和鉴别,采用柱前衍生化HPLCUV测定生物碱部位中总生物碱的含量。方法:采用HiQSiL C18色谱柱(4.6 mm×250 mm,5μm),以9-氯甲酸芴甲酯(FMOCCl)为柱前衍生化试剂,流动相乙腈-0.1%醋酸(50∶50),流速0.8 mL·min-1,检测波长254 nm,电喷雾离子源(ESI),正离子检测模式,以1-脱氧野尻霉素(DNJ)为对照,外标法计算桑叶总生物碱含量。结果:鉴定了6个生物碱类成分分别为DNJ,fagomine,3-epi-fagomine,DAB,calystegine B2和2-O-β-Glc-DAB;测定3批供试品中总生物碱含量均达到75%以上。结论:该法简便、准确、灵敏,可用于桑叶总生物碱及其制剂的定性定量分析。
OBJECTIVE: To analyze and identify the contents of alkaloids in the total alkaloids of mulberry leaves by HPLC-MS-MS. Pre-column derivatization HPLCUV was used to determine the contents of total alkaloids in alkaloids. METHODS: HiQSiL C18 column (4.6 mm × 250 mm, 5 μm) was used as the pre-column derivative of FMOCCl. The mobile phase was acetonitrile-0.1% acetic acid (50:50) mL · min-1, detection wavelength 254 nm, electrospray ionization (ESI), positive ion detection mode, and 1-deoxynojirimycin (DNJ) as control. RESULTS: Six alkaloids were identified as DNJ, fagomine, 3-epi-fagomine, DAB, calystegine B2 and 2-O-β-Glc-DAB. More than 75%. Conclusion: The method is simple, accurate and sensitive and can be used for qualitative and quantitative analysis of mulberry total alkaloids and their preparations.