GC-EI-MS法定性分析八角莲中鬼臼毒素成分

目的: 建立八角莲中鬼臼毒素成分GC-EI-MS的定性分析方法。 方法: 取八角莲的根茎粉末、胃组织(pH 3)用乙酸乙酯-正己烷(3∶ 1)提取,离心、浓缩,供GC-EI-MS法定性分析。气相色谱进样口温度为300 ℃,柱温从260 ℃经两步程度升温至315 ℃。质谱在m/z 41~500的范围内采用全扫描,采集时间为10~23 min。 结果: 鬼臼毒素成分最低检测限为0.002 mg·mL^-1(S/N≥3);添加鬼臼毒素对照品的平均回收率为86.73%,RSD＝7.2%(n＝5)。在八角莲的根茎粉末、饶某胃组织中均检出鬼臼毒素成分。 结论: 本测定方法可用于鬼臼毒素成分的定性分析。

Objective: To establish an effective GC-EI-MS method for analyzing the podophyllotoxin in Dysosma versipellis (Hance) M.Cheng ex Ying. Methods: Prior to the GC-EI-MS qualitative analysis,the stem-root from Dysosma versipelis (Hance) M.Cheng ex Ying,stomach tissue of the casualty(pH 3) from a casualty were extracted with ethyl acetate and n-hexane(3∶ 1,v/v) followed with centrifugation and concentration.The inlet temperature was set at 300 ℃ and the column temperature rose from 260 to 315 ℃ via a two-step temperature programmed.The MS data acquire from 10-23 min at the m/z range of 41-500 in the full scan mode. Results: The podophyllotoxin was detected with high sensitivity (0.002 mg·mL^-1) in so complex samples.The results showed good recovery rate(86.73%) with RSD of 7.2%.The podophyllotoxin was detected in both Mr.Rao's stomach tissue and the Dysosma versipellis (Hance) M.Cheng ex Yi stems and roots. Conclusion: The method is a simple,rapid,sensitive and accurate for the qualitative analysis of podophyllotoxin.