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GC/MS法同时检测无烟气烟草制品中的1,2-丙二醇、丙三醇和三甘醇

Simultaneous Determination of 1,2-Propylene Glycol,Glycerol and Triethylene Glycol in Smokeless Tobacco Products by Gas Chromatography-Mass Spectrometry

  • 摘要: 为了准确测定无烟气烟草制品中保润剂的含量,以14,-丁二醇为内标建立了同时检测无烟气烟草制品中1,2-丙二醇、丙三醇、三甘醇的气相色谱/质谱/选择离子监测(GC/MS/SIM)方法,采用该方法和CORESTA推荐的GC/FID法测定了30个无烟气烟草制品样品,并将2种方法的检测结果进行了比较。结果表明:①该方法的检出限和定量限分别为1.25~2.75μg/g和4.10~9.05μg/mL,回收率89.3%~100.3%,相对标准偏差(RSD)1.16%~4.37%;②所测无烟气烟草制品中1,2-丙二醇、丙三醇、三甘醇的含量分别在0.011~40.817,0.024~39.044和0.012~0.099 mg/g之间;③GC/FID法检出13个样品中含12,-丙二醇,检出率43.3%;14个样品中含丙三醇,检出率46.7%,其中能够准确定量的有9个样品;未检出三甘醇;④GC/MS/SIM法检出29个样品中含1,2-丙二醇,检出率96.7%,其中能够准确定量的有16个样品;28个样品中含丙三醇,检出率93.3%,其中能够准确定量的有25个样品;21个样品中含三甘醇,检出率70.0%,其中能够准确定量的有11个样品;⑤GC/FID和GC/MS/SIM法共同检出的13个样品中的12,-丙二醇含量和9个样品的丙三醇含量的皮尔逊(Pearson)相关系数均大于0.99,概率P值均小于显著性水平0.05,配对t检验概率P值均大于显著性水平0.05。结论:两种方法的定量结果一致,但GC/MS/SIM法灵敏度更高,定性更准确,GC/MS/SIM法更适合无烟气烟草制品中12,-丙二醇、丙三醇、三甘醇的定性定量分析。

     

    Abstract: A gas chromatography-mass spectrometry(GC/MS) method under selected ion monitoring(SIM) mode was developed for the simultaneous determination of 1,2-propylene glycol,glycerol and triethylene glycol in smokeless tobacco products(STPs) by using 1,4-butanediol as an internal standard.Thirty STP samples were parallel tested by GC/MS/SIM and GC/FID,a CORESTA recommended method,and the results were compared.The results showed that:1) The recoveries of 1,2-propylene glycol,glycerol and triethylene glycol ranged from 89.3% to 100.3% with the limits of detection of 1.25 to 2.75 μg/g and RSDs of 1.16% to 4.37%.2) The contents of 1,2-propylene glycol,glycerol,and triethylene glycol in the samples ranged from 0.011 to 40.817,0.024 to 39.044,0.012 to 0.099 mg/g,respectively.3)1,2-propylene glycol in 13 samples and glycerol in 14 samples were detected,and their contents in 9 of the samples were accurately determinable,however,triethylene glycol was undetectable in all samples by GC/FID.4)1,2-propylene glycol in 29 samples,glycerol in 28 samples and triethylene glycol in 21 samples were detected,their contents in 16,25 and 11 of the samples could be accurately determined by GC/MS/SIM method,respectively.5) The Pearson correlation coefficients between the contents of 1,2-propylene glycol in 13 samples and glycerol in 9 samples determined by GC/FID and GC/MS/SIM were over 0.99 probable value less than significant level of 0.05 and paired test t value over significant level of 0.05.It was concluded that the target analytes in the samples determined by GC/MS/SIM agreed with those by GC/FID,however,GC/MS/SIM method was more sensitive and accurate.GC/MS/SIM method is more suitable for the qualitative and quantitative determination of 1,2-propylene glycol,glycerol,and triethylene glycol in smokeless tobacco products.

     

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