固相萃取富集/气相色谱法测定烟草中的9种有机酸  

Determination of Organic Acids in Tobacco by Solid Phase Extraction and Gas Chromatogarphy

作　　者：张霞[1] 刘志华[1] 杨光宇[1] 杨柳[1] 段沅杏[1] 刘春波[1] 陈永宽[1] 缪明明[1] 

机构地区：[1]云南烟草科学研究院 云南省烟草化学重点实验室,云南昆明650106

出　　处：《分析测试学报》2014年第5期545-550,共6页Journal of Instrumental Analysis

基　　金：云南中烟公司科技项目基金资助(2012JC02);云南省烟草化学创新团队(2009CI014)

摘　　要：建立了用硫酸甲醇甲酯化衍生-固相萃取富集/气相色谱测定烟草中9种有机酸的方法,首次实现了强酸介质中有机酸酯的固相萃取.烟草样品用硫酸-甲醇进行甲酯化衍生,衍生生成的有机酸酯用MCI-GEL反相树脂分离富集,萃取液用甲醇洗脱后进行气相色谱分析,采用DB-5毛细管色谱柱,进样量1.0止,不分流进样;检测器温度250℃.方法可同时准确测定烟草样品中乳酸、草酸、丙二酸、乙酰丙酸、苹果酸、柠檬酸、棕榈酸、硬脂酸、亚油酸的含量,各有机酸的加标回收率为92.2％～102.6％,相对标准偏差为2.4％～3.2％。A new method for the determination of 9 organic acids in tobacco was developed by deri-vatization, solid phase extraction and gas chromatography（GC）. The tobacco samples were methyla-ted with methanol and sulfuric acid. The organic acid ester was firstly extracted using solid-phase ex-traction in strong acidic medium, and then enriched with MCI - GEL and eluted with methanol. Theeluent was determined by GC with a DB-5 capillary column and a splitless injection volume of 1.0 μL at a detector temperature of 250 %. This method was applied in the determination of lactic acid, ox-alic acid, propandioie acid, acetylpropionic acid, malic acid, citric acid, palmic acid, linoleicacid and stearic acid in tobacco samples. The recoveries were in the range of 92. 2% - 102.6% withrelative standard deviations （RSD） of 2.4% - 3.2%. The limits of quantitation （LOQ） for all ana-lytes were between 0. 20 mg/L and 0. 36 mg/L. The method was accurate and sensitive, and couldmeet the actual requirements for the

关 键 词：固相萃取 富集 气相色谱 烟草 有机酸 

分 类 号：O657.63[理学—分析化学]