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
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摘要
将2支剪碎的滤嘴(或1.000g卷烟烟丝)放入100mL锥形瓶中,加入40mL甲醇和80μL 50g·L~(-1)苯甲酸正丙酯内标溶液,80%超声功率条件下提取30min。取上清液,经0.45μm滤膜过滤后,以HP-INNOWAX色谱柱(30m×0.25mm,0.25μm)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10.0～400mg·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0.17mg·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。
Two chopped filters(or 1.000 g cut tobacco)were placed into a 100 mL conical bottle,and 40 mL of methanol and 80μL 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 0.45μm filtration membrane,and menthol in the supernatant was determined by gas chromatography-mass spectrometry with HP-INNOWAX column(30 m×0.25 mm,0.25μm)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 of10.0-400 mg·L~(-1),with detection limit(3 s)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%.
Two chopped filters(or 1.000 g cut tobacco)were placed into a 100 mL conical bottle,and 40 mL of methanol and 80μL 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 0.45μm filtration membrane,and menthol in the supernatant was determined by gas chromatography-mass spectrometry with HP-INNOWAX column(30 m×0.25 mm,0.25μm)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 of10.0-400 mg·L~(-1),with detection limit(3 s)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%.
引文
[1]WAYNE G F,CONNOLLY G N.Application,function,and effects of menthol in cigarettes:A survey of tobacco industry documents[J].Nicotine&Tobacco Research,2004,6(s1):43-54.
[2]宋瑜冰,谢剑平,宗永立,等.薄荷醇在卷烟中转移行为的控制及检测研究综述[J].香料香精化妆品,2005(3):25-28.
[3]蔡卫兵,朱鲜艳,曹传华.气相色谱法测定滤棒用薄荷香精中薄荷醇[J].理化检验-化学分册,2008,44(3):287-287.
[4]石先哲,何智慧,窦阿波,等.基于液相色谱-质谱联用技术的代谢组学方法研究薄荷烟对大鼠代谢的影响[J].色谱,2010,28(8):765-768.
[5]林文强,欧亚非,王瑞玲,等.薄荷型卷烟和主流烟气中薄荷醇分析及其转移的研究[J].化学研究与应用,2010,22(9):1122-1125.
[6]胡启秀,孙海峰,孔浩辉,等.气相色谱法测试卷烟烟气冷凝物中薄荷醇国际标准的研究[J].烟草科技,2013(5):56-60.
[7]YC/T 286-2009卷烟主流烟气中薄荷醇的测定气相色谱法[S].
[8]黄龙,陈一,刘辉,等.卷烟及烟气中薄荷醇的毛细管气相色谱分析[J].烟草科技,2007(4):32-35.
[9]YC/T 285-2009卷烟配方烟丝中薄荷醇的测定气相色谱法[S].
[10]YC/T 416-2011醋酸纤维滤棒中薄荷醇的测定气相色谱法[S].
[11]张卫平,陆明华,胡爱平,等.气相色谱法测定醋酸纤维滤棒中的薄荷醇[J].理化检验-化学分册,2014,50(10):1299-1302.
[12]CELEBUCKI C C,WAYNE G F,CONNOLLY GN,et al.Characterization of measured menthol in 48U.S.cigarette sub-brands[J].Nicotine&Tobacco Research,2005,7(4):523-531.
[13]游金清,朱钢添,张艳,等.顶空气相色谱法测定薄荷型卷烟中的薄荷醇[J].烟草科技,2014(8):51-54.
[14]刘立全,李维娜,王月侠,等.特殊滤嘴研究进展[J].烟草科技,2004(3):17-24.
[15]何智慧,罗嘉,练文柳.薄荷卷烟研究进展[J].烟草科技,2006(9):38-42.
[2]宋瑜冰,谢剑平,宗永立,等.薄荷醇在卷烟中转移行为的控制及检测研究综述[J].香料香精化妆品,2005(3):25-28.
[3]蔡卫兵,朱鲜艳,曹传华.气相色谱法测定滤棒用薄荷香精中薄荷醇[J].理化检验-化学分册,2008,44(3):287-287.
[4]石先哲,何智慧,窦阿波,等.基于液相色谱-质谱联用技术的代谢组学方法研究薄荷烟对大鼠代谢的影响[J].色谱,2010,28(8):765-768.
[5]林文强,欧亚非,王瑞玲,等.薄荷型卷烟和主流烟气中薄荷醇分析及其转移的研究[J].化学研究与应用,2010,22(9):1122-1125.
[6]胡启秀,孙海峰,孔浩辉,等.气相色谱法测试卷烟烟气冷凝物中薄荷醇国际标准的研究[J].烟草科技,2013(5):56-60.
[7]YC/T 286-2009卷烟主流烟气中薄荷醇的测定气相色谱法[S].
[8]黄龙,陈一,刘辉,等.卷烟及烟气中薄荷醇的毛细管气相色谱分析[J].烟草科技,2007(4):32-35.
[9]YC/T 285-2009卷烟配方烟丝中薄荷醇的测定气相色谱法[S].
[10]YC/T 416-2011醋酸纤维滤棒中薄荷醇的测定气相色谱法[S].
[11]张卫平,陆明华,胡爱平,等.气相色谱法测定醋酸纤维滤棒中的薄荷醇[J].理化检验-化学分册,2014,50(10):1299-1302.
[12]CELEBUCKI C C,WAYNE G F,CONNOLLY GN,et al.Characterization of measured menthol in 48U.S.cigarette sub-brands[J].Nicotine&Tobacco Research,2005,7(4):523-531.
[13]游金清,朱钢添,张艳,等.顶空气相色谱法测定薄荷型卷烟中的薄荷醇[J].烟草科技,2014(8):51-54.
[14]刘立全,李维娜,王月侠,等.特殊滤嘴研究进展[J].烟草科技,2004(3):17-24.
[15]何智慧,罗嘉,练文柳.薄荷卷烟研究进展[J].烟草科技,2006(9):38-42.