气-质联用(GC/MS)法测定烟草生物碱的方法优化

采用气相色谱-质谱法(GC/MS),通过优化相关技术参数建立了能够快速准确测定烟草中烟碱和微量生物碱(降烟碱、麦斯明、假木贼碱和新烟草碱)含量的方法.经正交试验确定了超声提取和有机溶剂萃取前处理方法的最佳条件,结果表明:烟碱、降烟碱、麦斯明和假木贼碱的线性范围分别为20～600、30～300、3.2～12、16～60mg/L,检测限分别为0.11、0.09、0.02和0.04mg/kg,回收率介于88.5%～105.4%,相对标准偏差(n=5)介于2.4%～9.2%.该方法具有检测烟草生物碱灵敏度高和重现性好的特点,且操作简便,解决了已有方法存在的生物碱各个组分提取不完全和含量极低的麦斯明检测效果不理想等问题.

An improvement of method for tobacco alkaloids determination by chromatography-mass spectrometry

A quick and efficient method for simultaneous determination of nicotine,nornicotine,myosmine,anabasine and anatabine by GC-MS was developed.The optimum conditions of ultrasonic extraction and organic solvent extraction were radicated by the orthogonal design and volume of the extraction solvent was optimized.Regression function,recovery and precision of the method were reviewed.The results show that the linear ranges of nicotine,nornicotine,myosmine and anabasine were 20-600,30-300,3.2-12 and 16-60 mg/L,respectively.and the detection limits were 0.11,0.09,0.02 and 0.04 mg/kg,respectively.The recoveries were in the range of 88.5%-105.4% and the method precisions were in the range of 2.4%-9.2%.The test shows that the method comes on with high sensitivity,good precision good reproductibilty and convenient operation.The method has solved the problerm that alkaloids extraction was imperfect and the myosmine detection was ineffective.