GC-MS内标法分析测定晒黄烟烟叶中5种生物碱的含量

Determination of Five Alkaloids in Sun-Cured Yellow Tobacco by Gas Chromatography-Mass Spectrometry with Internal Standard Method

建立了气相色谱-质谱联用法（GC-MS）测定晒黄烟烟叶中烟碱、降烟碱、新烟碱、麦斯明和假木贼碱含量的方法。样品采用5％的氢氧化钠溶液湿润静置15rain后，加入一级内标溶液作为萃取剂，加盖密封后超声提取并离心，取下层有机相干燥后采用GC-MS进行定量分析。烟碱、降烟碱、新烟碱、麦斯明和假木贼碱在校准曲线浓度范围内呈现良好的线性关系（r均大于0．99），其检出限分别为69．8、34．7、56．4、19．5、43．2ng／mL，定量限分别为232．7、124．7、188．0、65．0、144．0ng／mL，低中高三个浓度的加标回收率在91．5％—102．3％之间，相对标准偏差（RSD）均小于5．0％，该方法准确可靠、重现性好，运用该方法能快速分析测定晒黄烟烟叶中5种生物碱的含量。

A gas chromatography-mass spectrometry （GC-MS） method was established for the determination of nicotine, nornicotine, anatabine, myosmine and anabaseine in sun-cured yellow tobacco.The samples were soaked in a NaOH solution （5%） for 15 min. Adding the internal standard solution as the extraction agent, the sealed sample was extracted using ultrasonic irradiation. After centrifugation, taking the organic phase below for drying, the extracted sample solution can be injected directly into GC-MS for quantitative analysis. The organic phase atler drying was quantitatively analysed by GC-MS. Nicotine, nornicotine, anatabine, myosmine and anabaseine were showed a good linear relationship （r were greater than 0.99） within the scope of the concentration of standard curve. The limits of detection were 69.8, 34.7, 56.4, 19.5 and 43.2 ng/mL respectively. The limits of quantitation were 232.7, 124.7, 188.0, 65.0 and 144.0 ng/mL respectively. The average recoveries at three levels were in the range of 91.5%—102.3% with the relative standard deviations （RSD） less than 5.0%. The method is accurate, reliable and reproducible. This method can be used to determine rapidly the five kinds of alkaloid in sun-cured yellow tobacco samples.