气相色谱-质谱测定卷烟醋纤滤棒三乙酸甘油酯方法的构建

Establishment of GC/MS Method Determining Triacetin in Cellulose Acetate Filter Rod of Cigarette

【目的】探求卷烟醋纤滤棒三乙酸甘油酯简便、灵敏与高效的测定方法,为卷烟醋纤滤棒质量控制及烟气苯酚释放量的管控提供技术支撑。【方法】称取一定量的醋纤滤棒,采用内标-正十七烷的无水乙醇超声萃取后选择离子模式进行定量分析,构建气相色谱-质谱联用测定卷烟醋纤滤棒中三乙酸甘油酯的分析方法。【结果】优化后选择的色谱柱、萃取剂和超声萃取时间分别为强极性TG-WAXMS(30m×0.25mm×0.25μm)、无水乙醇和40min;气相色谱-质谱法(GC/MS)对不同浓度三乙酸甘油酯准溶液分析得到其回归别为0.08μg/mL和0.15μg/mL,方法的灵敏度较高;加标回收试验的三乙酸甘油酯回收率为97.0%~测定卷烟醋纤滤棒中三乙酸甘油酯的分析方法操作简便、灵敏、高效,适于卷烟醋纤滤棒中三乙酸甘油酯的测定。

【Objective】The simple,sensitive and efficient method for determining triacetin in cellulose acetate filter rod of cigarette is explored to provide the technological support for quality control of cigarette cellulose acetate filter rod and regulation of smoke phenol release amount.【Method】A certain amount of cellulose acetate filter rod is weighed and ultrasonic extracted with anhydrous ethanol of heptadecane(internal standard),ion pattern is selected to conduct quantitative analysis,and then GC/MS method for determining triacetin in cellulose acetate filter rod of cigarette is established.【Result】The optimized chromatographic column,extractant,ultrasonic extraction time is strongly polar TG-WAXMS(30 m×0.25 mm×0.25μm),anhydrous ethanol and 40 min respectively.The regression equation y=1.25562 x solution,the correlation coefficient is 0.9997 and the linear relationship is good.LOD and LOQ of triacetin are 0.08μg/mL and 0.15μg/mL respectively,and the method has high sensitivity.The recovery2.6%—6.5%,which is meet the demand of quantitative analysis.【Conclusion】The established GC/MS method determining triacetin in cellulose acetate filter rod of cigarette is featured with simple operation,sensitivity and efficiency,which is suitable for determining triacetin in cellulose acetate filter rod of cigarette.