Purity Assessment Of Ester Tobacco Additives By Mass Balance Approach And Quantitative Nuclear Magnetic Resonance Method

As the largest tobacco producing country in the world today,China has increasingly standardized the quality control of tobacco additives,and clearly regulated the types and limits of tobacco additives.As one of the common tobacco additives in tobacco packaging,the overuse of ester tobacco additives not only affect the smoking experience of consumers,but also affect their health.This study takes propyl acetate as an example to research on determination the purity of ester tobacco additives based on two different principles methods to ensure the reliability of the purity result.The main conclusions are as following:1.Determination the purity by mass balance approach(MBA):a method for the determination of propyl acetate by gas chromatography(GC)was established,and the GC purity of propyl acetate was determined to be 99.29%.Gas chromatography-mass spectrometry(GC-MS)was used to identify the structure-related impurities in propyl acetate,and four structure-related impurities including methanol,isopropanol,n-propanol,and 2-ethylhexanyl acetate were confirmed.The quantitative results of each impurity via external standard method were 1.31 mg/g,0.15 mg/g,0.71 mg/g,and 2.26 mg/g,respectively.In addition,the typical impurities in propyl acetate were qualitatively and quantitatively determined.Finally,the purity of propyl acetate was determined by MBA was 99.36%with the uncertainty of 0.015%(k=2).2.Removal on the trace water by adsorption:For water content in raw propyl acetate is high,measurement uncertainty in the process of introducing the main problem.In this paper removal on the trace water by adsorption in propyl acetate was studied,and the adsorption parameters were optimized.After adsorption process,the water content in propyl acetate reduced to not more than 100 ?g/g,and the structure-related impurities of methanol and isopropanol were almost removed.Finally,the purity of propyl acetate by mass balance approach increased from 99.36%to 99.63%,uncertainty is reduced from 0.015%to 0.008%(k=2).3.Determination the purity by quantitative nuclear magnetic resonance method(qNMR):In this paper,quantitative nuclear magnetic resonance method was used to determine the purity of high purity propyl acetate,and chooses methanol CRM as the internal standard material in this study.Finally,the purity of high purity propyl acetate was determined by quantitative nuclear magnetic resonance method to 99.61%with the uncertainty of 0.32%(k=2),which was consistent with the purity of mass balance approach and could be used as a reference method for determination of volatile organic compounds.In this study,mass balance approach(MBA)and quantitative nuclear magnetic method(qNMR)were used to determine the purity of ester tobacco additives.A general method for the analysis of impurities in volatile organic reagents was established,which laid a foundation for the development of reference material for tobacco additives and had practical significance for tobacco quality control.