介质碰撞萃取结合气相色谱法测定烟草及烟草制品中水分、1,2-丙二醇、丙三醇和烟碱的含量  

Determination of Moisture,1,2-Propylene Glycol,Glycerol and Nicotine in Tobacco and Tobacco Products by Gas Chromatography with Medium Collision Extraction

作　　者：梁秋菊 王志国 杜文 刘巍 尹新强 卢红梅[2] LIANG Qiuju;WANG Zhiguo;DU Wen;LIU Wei;YIN Xinqiang;LU Hongmei(Technology Center of China Tobacco Hunan Industrial Co.,Ltd.,Changsha 410007,China;College of Chemistry and Chemical Engineering,Central South University,Changsha 410083,China)

机构地区：[1]湖南中烟工业有限责任公司技术中心,长沙410007 [2]中南大学化学化工学院,长沙410083

出　　处：《理化检验（化学分册）》2022年第12期1372-1379,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：湖南中烟工业有限责任公司博士后项目(KY2019JC0028)。

摘　　要：测定传统卷烟中水分、1,2-丙二醇、丙三醇和烟碱的行业标准已经不适用于新型卷烟产品。为开发适用于全品类烟草及烟草制品中水分、1,2-丙二醇、丙三醇和烟碱的测定方法,提出了以含6.5 g·L^(-1)异丙醇(水分的内标)、2.5 g·L^(-1)1,4-丁二醇(1,2-丙二醇和丙三醇的内标)和4.0 g·L^(-1)正十七烷(烟碱的内标)的体积比为100∶15的甲醇-三乙胺混合液为萃取剂的介质碰撞萃取结合气相色谱的分析方法。取烟草样品0.4000 g,不需要破碎处理,置于15 mL离心管中,加入10 mL萃取剂,在线速率为4 m·s-1的条件下室温处理2 min,静置3 min,取上清液过0.22μm有机系滤膜后进行气相色谱分析。结果表明:介质碰撞萃取前处理方法只需要2 min即可实现对烟草及烟草制品中4种主要成分的完全提取。水分标准曲线的线性范围在10.00 g·L^(-1)以内,1,2-丙二醇、丙三醇、烟碱标准曲线的线性范围在5.00 g·L^(-1)以内,检出限(3s)为0.030~0.35 mg·g^(-1)。对同一样品进行日内精密度(n=6)和日间精密度(n=8)试验,测定值的相对标准偏差小于4.0%。按照标准加入法进行回收试验,回收率为95.2%~100%。The industry standards of determination of moisture,1,2-propylene glycol,glycerol and nicotine in traditional cigarettes were no longer applicable to new type tobacco products.In order to develop a method suitable for the determination of moisture,1,2-propylene glycol,glycerol and nicotine in all kinds of tobacco and tobacco products,a method of gas chromatography with medium collision extraction was proposed using a mixture of methanol and triethylamine at volume ratio of 100∶15 containing 6.5 g·L^(-1)isopropanol(internal standard of water),2.5 g·L^(-1)1,4-butanediol(internal standard of 1,2-propylene glycol and glycerol)and 4.0 g·L^(-1)n-heptadecane(internal standard of nicotine)as extraction solvent.0.4000 g of tobacco sample was taken,which did not need to be broken,and placed into a 15 mL-centrifuge tube.And 10 mL of extraction solvent was added.The extraction was carried out under the linear velocity of 4 m·s-1for 2 min at room temperature,settling for 3 min.The supernatant was filtered through 0.22μm organic filter membrane,and then determined by gas chromatography.As shown by the results,the 4 main components in tobacco and tobacco products could be completely extracted in only 2 min by the pretreatment method of medium collision extraction.Linear range of moisture standard curve was within 10.00 g·L^(-1),while linear ranges of the standard curves of 1,2-propylene glycol,glycerol and nicotine were within 5.00 g·L^(-1),with detection limits(3s)of 0.030-0.35 mg·g^(-1).Tests for intra-day precision(n=6)and inter-day precision(n=8)were carried out on the same sample,with RSDs of determined values less than 4.0%.Test for recovery was made by standard addition method,giving results in the range of 95.2%-100%.

关 键 词：烟草及烟草制品 介质碰撞萃取 气相色谱法 水分 1 2-丙二醇 丙三醇 烟碱 

分 类 号：O657.7[理学—分析化学]