摘要
目的:用气相色谱-质谱联用法分析山豆根中生物碱类成分。方法:用索氏提取器以80%乙醇提取山豆根,碱性条件下二氯甲烷萃取,毛细管气相色谱-质谱检测,NBS 图谱库检索。色谱条件:BPX-5交联弹性石英毛细管柱(30 m×0.22 mm,0.25 μm),柱温:初始温度35℃(1 min)(40℃·min^(-1))→220℃(0 min)3℃·min^(-1)→280℃(10 min),MS 检测器,进样量1μL,载气 He(1.6 mL·min^(-1))。质谱条件:电离方式 EI,电子能量70 eV,源温180℃。结果:检测到15种苦参碱的异构体、3种氧化苦参碱的异构体、2种金雀花碱的异构体和 N-甲基金雀花碱,其中苦参碱是山豆根中的主要生物碱。结论:(1)本法简单可行,适用于中草药生物碱的定性测定;(2)碱性条件下,直接用二氯甲烷萃取,苦参碱的提取效率最高。
Objective：To apply GC - MS for analyzing alkaloids in Radix Sophorae Tonkinensis. Methods： Radix Sophorae Tonkinensis（Shandougen） was extracted in Soxhlet extraction apparatus with ethanol （80%）, after distilling ethanol,the solution was condensed on a rotary evaporator,and extracted by CH2Cl2 ,then separated by capillary gas chromatography and detected by mass spectrometry, the alkaloids were identified with their mass spectrum searched in NBS library. The gas chromatographic determinations were run on an Agilent 6890N using a BPX - 5 capillary column excellence（30 m×0. 22mm,film thickness0. 25 μm）. The carrying gas was helium with a flow rate of 1.6 mL · min^- 1. The oven temperature was programmed from 35 ℃ （ 1 min） to 220 ℃ （ 0 min） at 40 ℃ · min^- 1and then 220 ℃ to 280 ℃ （10 min） at 3 ℃· min^- 1. The mass spectrometer conditions were as follow：the ionization mode was EI ,ionization potential,70 eV. The source temperature, 180 ℃ and resolution, 1000. Result： 15 isomers of matrine,3 isomers of oxymatrine,2 isomers of cytisine and N- methylcytisine were detected,and matrine was the main alkaloid in Radix Sophorae Tonkinensis. Conclusions： （ 1 ） The method is simple, practical and reliable, it can be used to identify alkaloids in Chinese traditional herbs;（2 ）Matrine is extracted most effectively when dichlormethane is used as extractant in basic conditions.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第1期45-47,共3页
Chinese Journal of Pharmaceutical Analysis
关键词
山豆根
生物碱
气-质联用
Radix Sophorae Tonkinensis
alkaloids
GC - MS
