作　　者： ; ; ; ; ;

机构地区： 国家烟草质量监督检验中心

出　　处： 《烟草科技》 2014年第1期49-52,共4页

摘　　要： 为准确测定卷烟烟丝中的1，2-丙二醇、丙三醇及三甘醇，建立了分散固相萃取-气相色谱-质谱联用法（d．SPE—GC／MS）检测的分析方法。卷烟烟丝中的3种保润剂经甲醇振荡提取、N-丙基乙二胺粉末和无水硫酸镁分散固相萃取净化后进行GC／MS测定，采用内标法定量。结果表明：3种保润剂在0．0200～3．240mg／mL内线性关系良好（R2〉0．999），3个加标水平的回收率在97．4％～113．1％之间，平均相对标准偏差（RSD）小于7％，检出限（LOD）为2．27～22．80μg／g。4家实验室对6个样品的协同实验结果经柯克伦（Cochran）和格拉布斯（Grubbs）检验，实验室内重复性变异系数在2．3％～6．7％之间，实验室间再现性变异系数在4．7％～16．5％之间。该方法适合用于卷烟烟丝中1，2-丙二醇、丙三醇及三甘醇的测定。 In order to accurately determine 1,2-propylene glycol, glycerol and triethylene glycol in cigarette filler, a dispersive solid-phase extraction-gas chromatography-mass spectrometry （d-SPE-GC/MS） method was developed. The humectants in cigarette filler were extracted by mechanically shaking with methanol, and the extraction was cleaned up by primary-secondary amine （PSA） and MgSO4 based d-SPE before GC/MS analysis and subsequently quantified with an internal standard method. The results showed that： The three humectants possessed good linear correlation （R2 more than 0.999） within 0.0200-3.240 mg/mL, the average spiked recoveries ranged from 97.4% to 113.1% with the relative standard deviation lower than 7% and the limits of detection （LOD） from 2.27 to 22.80 μg/g. The coefficients of variation of intra-laboratory repeatability ranged from 2.3% to 6.7% and that of inter-laboratory reproducibility from 4.7% to 16.5%, through Cochran＇s Test and Grubbs＇ Test of experimental data from 4 laboratories and 6 test samples. This method is suitable for the simultaneous determination of 1,2-propylene glycol, glycerol and triethylene glycol in cigarette filler.

关 键 词： 气相色谱一质谱联用 分散固相萃取 保润剂 卷烟烟丝

领　　域： [农业科学] [轻工技术与工程]