GC-EI-MS法定性分析八角莲中鬼臼毒素成分  

GC-EI-MS qualitative analysis of podophyllotoxin in Dysosma versipellis (Hance) M. Cheng ex Ying

作　　者：段韵[1] 胡开发 王洪宗[3] 饶小平 刘勇孜[3] 张娜珍 

机构地区：[1]江西省人民医院药剂科,南昌330006 [2]抚州市临川公安分局,抚州344000 [3]江西省公安厅刑科所,南昌330006 [4]江西公安专科学校,南昌330009

出　　处：《药物分析杂志》2011年第8期1575-1578,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：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(pH3)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/z41～500的范围内采用全扫描,采集时间为10～23 m in。结果:鬼臼毒素成分最低检测限为0.002mg.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.

关 键 词：八角莲(六角莲) 鬼臼毒素 气相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]