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    超声提取-气相色谱-质谱法测定薄荷型卷烟烟丝及滤嘴中薄荷醇的含量

    Determination of Menthol in Cut Tobacco and Cigarette Filters of Mentholated Cigarettes by GC-MS with Ultrasonic Extraction

    • 摘要: 将2支剪碎的滤嘴(或1.000 g卷烟烟丝)放入100 mL锥形瓶中,加入40 mL甲醇和80 μL 50 g·L-1苯甲酸正丙酯内标溶液,80%超声功率条件下提取30 min。取上清液,经0.45 μm滤膜过滤后,以HP-INNOWAX色谱柱(30 m×0.25 mm,0.25 μm)为固定相,采用气相色谱-质谱法测定其中薄荷醇的含量。质谱分析中采用电子轰击离子源,全扫描和选择离子监测模式。薄荷醇的质量浓度在10.0~400 mg·L-1内与对应的峰面积和内标峰面积的比值呈线性关系,检出限(3s)为0.17 mg·L-1。对卷烟烟丝和滤嘴样品分别进行组内、组间精密度试验,测定值的相对标准偏差(n=5)均小于5.0%。按标准加入法进行回收试验,回收率在94.0%~101%之间。

       

      Abstract: Two chopped filters (or 1.000 g cut tobacco) were placed into a 100 mL conical bottle, and 40 mL of methanol and 80 μL of 50 g·L-1 n-propyl benzoate solution for internal standard were added. After extraction for 30 min under 80% ultrasonic power, the supernatant was filtered with 0.45 μm filtration membrane, and menthol in the supernatant was determined by gas chromatography-mass spectrometry with HP-INNOWAX column (30 m×0.25 mm, 0.25 μm) as stationary phase. Electron bombardment ion source, full scanning mode and selective ion monitoring mode were adopted in mass spectrometry. Linear relationship between values of the ratio of menthol peak area to internal standard peak area and mass concentration of menthol was obtained in the range of 10.0-400 mg·L-1, with detection limit (3s) of 0.17 mg·L-1. Tests of intra and inter group precision for cut tobacco and cigarette filters were made, and values of RSDs (n=5) were all less than 5.0%. Test for recovery was made by standard addition method, giving results in the range of 94.0%-101%.

       

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