气相色谱法同时检测加热不燃烧卷烟芯材中的1,2-丙二醇、烟碱与甘油含量
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摘要
为准确测量加热不燃烧卷烟芯材中的1,2-丙二醇、烟碱与甘油含量,将加热不燃烧卷烟芯材样品切丝,以1,4丁二醇、正十七碳烷为内标,异丙醇内标溶液振荡萃取2 h,建立气相色谱法同时测定1,2-丙二醇、烟碱和甘油含量,并利用卡尔费休水分电位滴定仪检测样品中水分,计算得到样品中1,2-丙二醇、烟碱和甘油的绝干含量。结果表明1,2-丙二醇、烟碱、甘油分别在1.0～10.0 mg/mL、0.1～1.0 mg/mL、1.0～10.0 mg/mL范围内,工作曲线线性良好,相关系数均高于0.999,相对标准偏差分别为1.50%、2.62%、0.70%,加标回收率在97.11%～102.62%之间,检出限分别为0.019 mg/mL、0.009 mg/mL、0.011 mg/mL,定量限分别为0.064 mg/mL、0.030 mg/mL、0.039 mg/mL。该方法前处理简单、安全,定量结果准确可靠、重现性好,适用于加热不燃烧卷烟芯材中1,2-丙二醇、烟碱、甘油定量分析。
In order to accurately determine the content of 1,2-propylene glycol, nicotine and glycerol in heatnot-burn cigarette core material, an analysis method was developed by gas chromatography. 1,4-butanediol,and n-heptadecane as double internal standards. Samples were oscillatory extracted for 2 h by isopropanol solution and detected by GC. Meanwhile using volumetric KF moisture titrator detected the moisture of samples, then calculated the absolute dry content of 1,2-propylene glycol, nicotine and glycerol of samples.The results showed that the calibration curves of 1,2-propylene glycol, nicotine and glycerol is liner, in the range of 1.0-10.0 mg/mL, 0.1-1.0 mg/mL and 1.0-10.0 mg/mL, r2 were higher than 0.999 and RSD respectively were 1.50%, 2.62%, 0.70%. Spike recovery was between 97.11%-102.62%. The limits of detection(LOD)were 0.019 mg/mL, 0.009 mg/mL and 0.011 mg/mL. The limits of quantification(LOQ) were 0.064 mg/mL,0.030 mg/mL and 0.039 mg/mL. This method is simple, safe, accurate and good reproducibility of quantitative results, suiting for quantitative analysis of 1,2-propylene glycol, nicotine and glycerol in heat-not-burn tobacco products.
In order to accurately determine the content of 1,2-propylene glycol, nicotine and glycerol in heatnot-burn cigarette core material, an analysis method was developed by gas chromatography. 1,4-butanediol,and n-heptadecane as double internal standards. Samples were oscillatory extracted for 2 h by isopropanol solution and detected by GC. Meanwhile using volumetric KF moisture titrator detected the moisture of samples, then calculated the absolute dry content of 1,2-propylene glycol, nicotine and glycerol of samples.The results showed that the calibration curves of 1,2-propylene glycol, nicotine and glycerol is liner, in the range of 1.0-10.0 mg/mL, 0.1-1.0 mg/mL and 1.0-10.0 mg/mL, r2 were higher than 0.999 and RSD respectively were 1.50%, 2.62%, 0.70%. Spike recovery was between 97.11%-102.62%. The limits of detection(LOD)were 0.019 mg/mL, 0.009 mg/mL and 0.011 mg/mL. The limits of quantification(LOQ) were 0.064 mg/mL,0.030 mg/mL and 0.039 mg/mL. This method is simple, safe, accurate and good reproducibility of quantitative results, suiting for quantitative analysis of 1,2-propylene glycol, nicotine and glycerol in heat-not-burn tobacco products.
引文
[1]窦玉青,沈轶,杨举田,等.新型烟草制品发展现状及展望[J].中国烟草科学,2016-10,37(5):92-97.
[2]李翔,谢复炜,刘惠民.新型烟草制品毒理学评价研究进展[J].烟草科技,2016,49(1):88-93.
[3]FOY J W D,BOMBICK B R,BOMBICK D W,et al.Acomparison of in vitro toxicities of cigarette smoke condensate from“Eclipse”cigarettes and four commercially available ultralow-“tar”cigarettes[J].Food and Chemical Toxicology,2004,42(2):237-243.
[4]洪群业,郑路,程多福,等.国内加热不燃烧型卷烟专利技术统计分析[J].烟草科技,2017,50(11):66-74.
[5]王孝峰,周顺,何庆,等.加热状态下烟草气溶胶释放特性的影响因素:温度、甘油和气氛[J].烟草科技,2017,50(10):48-54.
[6]朱浩,席辉,柴国璧,等.温度对加热非燃烧卷烟烟熏香成分释放的影响[J].烟草科技,2017,50(11):33-38.
[7]赵龙,刘珊,曾世通,等.甘油对烟丝加热状态下烟气中挥发性和半挥发性成分的影响[J].烟草科技,2016,49(4):53-60.
[8]刘珊,崔凯,曾世通,等.加热非燃烧型烟草制品剖析[J].烟草科技,2016,49(11):56-65.
[9]谢剑平.烟草与烟气化学成分[M].北京:化学工业出版社,2011:365.
[10]左萍,吴军武,许立宪,等.气相色谱法同时测定牙膏中二甘醇,丙二醇,甘油[J].检验检疫科学,2008,18(4):46-48.
[11]王岚,李忠,蒋次清,等.HPLC法同时测定烟草和料液中的糖和保润剂[J].烟草科技,2006(8):25-28.
[12]黄菲,黄翼飞.高效液相色谱测定烟用香精及料液中保润剂方法的改进[J].现代食品科技,2011,27(8):1043-1046.
[13]段沅杏,吴亿勤,杨威,等.GC/MS法同时测定电子烟烟气释放物中的5种醇类化合物[J].烟草科技,2015,48(10):43-47,61.
[14]Determination of 1,2-propylene glycol and glycerol in tobacco and tobacco products by gas chromatography:CORESTARecommended Methods No.60[S].2005.
[15]Determination of 1,2-propylene glycol,glycerol and sorbitol in tobacco and tobacco products by high performance liquid chromatography(HPLC):CORESTA Recommended Methods No.61[S].2005.
[16]烟草及烟草制品1,2-丙二醇、甘油的测定气相色谱法:YC/T243-2008[S].北京:中国标准出版社,2008.
[17]烟用香精乙醇、1,2-丙二醇、甘油含量测定气相色谱法:YC/T 242-2008[S].北京:中国标准出版社,2008.
[18]烟草及烟草制品1,2-丙二醇、甘油和山梨醇的测定高效液相色谱法:YC/T 244-2008[S].北京:中国标准出版社,2008.
[19]段沅杏,赵伟,杨威,等.口用型无烟气烟草制品中烟碱的测定[J].烟草科技,2017,50(7):69-75.
[20]吴亿勤,刘秀明,秦云华,等.DART-MS/MS法测定烟草及烟草制品中的烟碱[J].烟草科技,2017,50(8):46-51,74.
[21]邓小华,陈冬林,周冀衡,等.湖南烤烟烟碱含量空间分布特征及与香吃味的关系[J].中国烟草科学,2009,30(5):34-40.
[22]烟草及烟草制品烟碱的测定气相色谱法:YC/T246-2008[S].北京:中国标准出版社,2008.
[23]卷烟总粒相物中烟碱的测定气相色谱法:GB/T 23355-2009[S].北京:中国标准出版社,2009.
[24]蔡君兰,刘绍锋,陈黎,等.一种电子烟烟液中烟碱、丙二醇和甘油的同时测定方法:201510122472.9[P].2015-05-27.
[25]蔡君兰,陈黎,彭斌,等.气相色谱法同时测定电子烟烟液中的烟碱、1,2-丙二醇和甘油[J].中国烟草学报,2016,22(5):1-9.
[26]烟草及烟草制品水分的测定卡尔费休法:GB/T 23357-2009[S].北京:中国标准出版社,2009.
[2]李翔,谢复炜,刘惠民.新型烟草制品毒理学评价研究进展[J].烟草科技,2016,49(1):88-93.
[3]FOY J W D,BOMBICK B R,BOMBICK D W,et al.Acomparison of in vitro toxicities of cigarette smoke condensate from“Eclipse”cigarettes and four commercially available ultralow-“tar”cigarettes[J].Food and Chemical Toxicology,2004,42(2):237-243.
[4]洪群业,郑路,程多福,等.国内加热不燃烧型卷烟专利技术统计分析[J].烟草科技,2017,50(11):66-74.
[5]王孝峰,周顺,何庆,等.加热状态下烟草气溶胶释放特性的影响因素:温度、甘油和气氛[J].烟草科技,2017,50(10):48-54.
[6]朱浩,席辉,柴国璧,等.温度对加热非燃烧卷烟烟熏香成分释放的影响[J].烟草科技,2017,50(11):33-38.
[7]赵龙,刘珊,曾世通,等.甘油对烟丝加热状态下烟气中挥发性和半挥发性成分的影响[J].烟草科技,2016,49(4):53-60.
[8]刘珊,崔凯,曾世通,等.加热非燃烧型烟草制品剖析[J].烟草科技,2016,49(11):56-65.
[9]谢剑平.烟草与烟气化学成分[M].北京:化学工业出版社,2011:365.
[10]左萍,吴军武,许立宪,等.气相色谱法同时测定牙膏中二甘醇,丙二醇,甘油[J].检验检疫科学,2008,18(4):46-48.
[11]王岚,李忠,蒋次清,等.HPLC法同时测定烟草和料液中的糖和保润剂[J].烟草科技,2006(8):25-28.
[12]黄菲,黄翼飞.高效液相色谱测定烟用香精及料液中保润剂方法的改进[J].现代食品科技,2011,27(8):1043-1046.
[13]段沅杏,吴亿勤,杨威,等.GC/MS法同时测定电子烟烟气释放物中的5种醇类化合物[J].烟草科技,2015,48(10):43-47,61.
[14]Determination of 1,2-propylene glycol and glycerol in tobacco and tobacco products by gas chromatography:CORESTARecommended Methods No.60[S].2005.
[15]Determination of 1,2-propylene glycol,glycerol and sorbitol in tobacco and tobacco products by high performance liquid chromatography(HPLC):CORESTA Recommended Methods No.61[S].2005.
[16]烟草及烟草制品1,2-丙二醇、甘油的测定气相色谱法:YC/T243-2008[S].北京:中国标准出版社,2008.
[17]烟用香精乙醇、1,2-丙二醇、甘油含量测定气相色谱法:YC/T 242-2008[S].北京:中国标准出版社,2008.
[18]烟草及烟草制品1,2-丙二醇、甘油和山梨醇的测定高效液相色谱法:YC/T 244-2008[S].北京:中国标准出版社,2008.
[19]段沅杏,赵伟,杨威,等.口用型无烟气烟草制品中烟碱的测定[J].烟草科技,2017,50(7):69-75.
[20]吴亿勤,刘秀明,秦云华,等.DART-MS/MS法测定烟草及烟草制品中的烟碱[J].烟草科技,2017,50(8):46-51,74.
[21]邓小华,陈冬林,周冀衡,等.湖南烤烟烟碱含量空间分布特征及与香吃味的关系[J].中国烟草科学,2009,30(5):34-40.
[22]烟草及烟草制品烟碱的测定气相色谱法:YC/T246-2008[S].北京:中国标准出版社,2008.
[23]卷烟总粒相物中烟碱的测定气相色谱法:GB/T 23355-2009[S].北京:中国标准出版社,2009.
[24]蔡君兰,刘绍锋,陈黎,等.一种电子烟烟液中烟碱、丙二醇和甘油的同时测定方法:201510122472.9[P].2015-05-27.
[25]蔡君兰,陈黎,彭斌,等.气相色谱法同时测定电子烟烟液中的烟碱、1,2-丙二醇和甘油[J].中国烟草学报,2016,22(5):1-9.
[26]烟草及烟草制品水分的测定卡尔费休法:GB/T 23357-2009[S].北京:中国标准出版社,2009.