气相色谱测定烟草中非挥发有机酸方法改进  

Improvement of the analysis method for non-volatile organic acids in tobacco by gas chromatography

作　　者：刘瑞红 潘立宁[1] 王晓瑜[1] 陈黎[1] 陈满堂 秦亚琼[1] 刘克建[1] 王冰[1] 谢复炜[1] LIU Ruihong;PAN Lining;WANG Xiaoyu;CHEN Li;CHEN Mantang;QIN Yaqiong;LIU Kejian;WANG Bing;XIE Fuwei(Zhengzhou Tobacco Research of CNTC,Zhengzhou 450001,China)

机构地区：[1]中国烟草总公司郑州烟草研究院,郑州450001

出　　处：《化学分析计量》2022年第12期22-28,共7页Chemical Analysis And Meterage

基　　金：国家烟草专卖局科技重点研发项目(110202002003)。

摘　　要：对烟草有机酸硫酸甲醇衍生化条件及萃取条件进行改进和优化,设计一种重复性好、萃取效率高、测定步骤少且对气相色谱仪损耗小的烟草样品处理方法。结果表明,样品在80℃水浴条件下经5%硫酸–甲醇衍生回流120 min后,利用磷酸氢二钠–氯化钠混合盐水溶液的盐析作用,经分液漏斗振荡萃取2次,并通过己二酸和十九酸双内标定量,由气相色谱–火焰离子检测法可成功分离和定量检测烟草中13种重要的非挥发有机酸。该方法测定有机酸具有良好的线性,相关系数均大于0.999,测定结果的相对标准偏差不大于3.5%(n=10),平均加标回收率为90.6%~105.0%,定量限为0.02~0.13 mg/g。The sulfuric acid methanol derivatization conditions and extraction conditions of tobacco organic acids were improved and optimized, and a method with good repeatability, high extraction efficiency, less determination steps and less damage to gas chromatography was designed. The results showed that the sample was heated to reflux for 120 min with5% sulfuric acid-methanol as derivatization reagent under 80 ℃, and followed by salting out with Na2HPO4-NaCl solution and extraction twice in a separatory funnel, the 13 non-volatile organic acids were simultaneously determined by GC-FID,using adipic acid and nonadenic acid as dual internal standards. This method had good linearity with the corelation coefficient more than 0.999, the relative standard deviation was 3.5%(n=10), the average recovery rates were 90.6%-105.0%, and the quantification limit was 0.02-0.13 mg/g.

关 键 词：非挥发性有机酸 甲酯化 盐析萃取 气相色谱–火焰离子检测 

分 类 号：TS411[农业科学—烟草工业]