微波辅助提取-气相色谱-质谱法测定石蒜中加兰他敏和力可拉敏

GC-MS Determination of Galanthamine and Lycoramine in Bulb of Lycoris Radiata with Microwave Assisted Extraction

采用乙醇(95+5)溶液于70℃提取石蒜中加兰他敏和力可拉敏,所得提取液经过滤后旋转蒸发至干。残渣溶于盐酸(2+98)溶液中,用氯仿萃取3次以除去杂质,用氨水调节水相酸度至pH 10,再用氯仿萃取3次,合并萃取液并蒸发至干。用甲醇溶解残渣,所得溶液用DB-5MS毛细管柱分离,进样量为1μL。质谱分析中采用电子轰击离子源及在(m/z)50～550范围内全扫描方式检测。检索图谱库NBS 75K.L及NIST 147对样品作定性分析,并根据[M^+]286及[M^+]288的丰度分别对加兰他敏和力可拉敏作定量分析。对方法做回收及精密度试验,测得回收率在93.0%～106.0%之间,相对标准偏差(n=9)为5.5%(加兰他敏)和2.4%(力可拉敏)。

Galanthamine （GLTM） and lycoramine （LCRM） were extracted from the sample of bulbs of Lycoris radiata with ethyl alcohol（95＋5） under 70 ℃. The extract obtained was filtered and evaporated to dryness with a rotary evaporator. The residue was dissolved with HCI（2＋98） and extracted thrice with CHCl3 to remove impurities. The aqueous phase was adjusted to pH 10 with aq. ammonia and extracted thrice with CHCI3 again. The organic phase was collected and evaporated to dryness. The residue was dissolved with methanol and DB-5MS capillary column was used for separation. OneμL was taken as volume of .sample introduction. Electron ionization and full-scanning in the range from （m/z） 50 to 550 were adopted in MS analysis. Qualitative analysis was performed by referring to the spectra database of NBS 75K L and NIST 147. Quantitative analysis was carried out with [M＋ ] 286 and [M＋ ] 288 for GLTM and LCRM respectively. Tests for recovery and precision were made, giving results of recovery ranged from 93. 0% to 106. 0%and RSD＇s （n=9） of 5. 5%（for GLTM） and 2. 4% （for LCRM）.