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    气相色谱-质谱法测定胶基型嚼烟中烟碱的含量

    GC-MS Determination of Nicotine in Gum Chewing Tobacco

    • 摘要: 取(1.42±0.01)g的试样5粒,溶解在5 mol·L-1氢氧化钠溶液8 mL和含内标的正己烷40 mL中,磁力搅拌110 min,静置20 min。取上层萃取液2 mL,用无水硫酸钠干燥,过0.22 μm有机相滤膜。所得溶液采用DB-5MS色谱柱进行气相色谱分离。质谱分析采用选择离子监测模式。烟碱的线性范围为4.00~200 mg·L-1,检出限(3s)为0.19 mg·L-1。按标准加入法进行回收试验,回收率在91.0%~96.1%之间,测定值的相对标准偏差(n=6)均小于3.0%。

       

      Abstract: 5 pellets of the sample of (1.42±0.01) g were dissolved with 8 mL of 5 mol·L-1 sodium hydroxide solution and 40 mL of hexane containing internal standard substance. The solution was magnetically stirred for 110 min, and stood for 20 min. An aliquot of 2 mL of the extract from the upper layer was dried with anhydrous sodium sulfate, and filtered through organic filter membrane of 0.22 μm. The sample solution was separated by GC using DB-5MS chromatographic column. SIM was adopted in MS analysis. Linearity range of nicotine was 4.00-200 mg·L-1, with detection limit (3s) of 0.19 mg·L-1. Test for recovery was made by standard addition method, giving results in the range of 91.0%-96.1%, with RSDs (n=6) all less than 3.0%.

       

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