GC-MS法分析烟用香精中10种有机酸  

Analysis of ten organic acids in tobacco flavors by gas chromatography-mass spectrometry

作　　者：汤晓东[1] 苏燕[1] 张丽娜[1] 陈晓水[1] 蒋佳磊[1] 朱书秀[1] 杨君[1] TANG Xiaodong;SU Yan;ZHANG Lina;CHEN Xiaoshui;JIANG Jialei;ZHU Shuxiu;YANG Jun(Technology Center of China Tobacco Zhejiang Industrial Co.,Ltd.,Hangzhou 310024,China)

机构地区：[1]浙江中烟工业有限责任公司技术中心,杭州市310024

出　　处：《烟草科技》2021年第4期49-56,共8页Tobacco Science & Technology

基　　金：浙江中烟工业有限责任公司科技项目“烟用香精中非挥发性有机酸检测方法的建立及其应用研究”(ZJZY2021C007)。

摘　　要：为实现烟用香精中有机酸的分离和测定,通过优化实验条件,建立了气相色谱-质谱(GC-MS)测定草酸、丙二酸、琥珀酸、苹果酸、棕榈酸、柠檬酸、硬脂酸、油酸、亚油酸和亚麻酸的方法。样品在室温下经10%(体积分数)硫酸甲醇溶液衍生24 h,然后用二氯甲烷萃取,并在选择离子模式(SIM)下进行GC-MS分析,采用己二酸为内标进行定量。结果表明:(1)在优化条件下,目标物在各自线性范围内线性关系良好(回归方程的R2均大于0.998),检出限和定量限分别在0.004~0.080和0.013~0.267 mg/kg之间,加标回收率在83.06%~110.29%之间,相对标准偏差在1.01%~6.50%之间。(2)利用该方法对26个烟用香精样品进行分析,发现10种有机酸在绝大多数样品中均有检出,且其质量分数在加香香精和加料香精中差异明显。(3)该方法操作简便,灵敏度和精密度高,适用于批量分析香精中10种有机酸的质量分数。In order to accomplish the separation and determination of organic acids in tobacco flavors,a gas chromatography-mass spectrometry(GC-MS)method for the determination of oxalic acid,malonic acid,succinic acid,malic acid,palmitic acid,citric acid,stearic acid,oleic acid,linoleic acid and linolenic acid was developed by optimized the experimental conditions.The samples were derived with a 10%sulfuric acid-methanol(V/V)solution at room temperature for 24 hours,and then extracted with dichloromethane.The derived samples were analyzed by GC-MS under SIM mode and quantified by using adipic acid as internal standard.The results showed that:(1)Under the optimized conditions,the linear relationships of the target compounds in the respective linear ranges(R2>0.998)were good,and the detection limits and quantification limits were in the ranges of 0.004-0.080 and 0.013-0.267 mg/kg respectively.The spiked recoveries of this method ranged from 83.06%to 110.29%with RSDs of 1.01%-6.50%.(2)Tobacco flavor samples of 26 kinds were analyzed using the developed method,it was found that the above ten organic acids were detected in most of the samples,and their contents in the flavors and those for casing were significantly different.(3)With the advantages of easy operation and higher sensitivity and precision,this method was suitable for the analysis of the ten organic acids in flavor samples.

关 键 词：烟草 加香香精 加料香精 气相色谱-质谱 有机酸 衍生化 

分 类 号：TQ657.4[化学工程—精细化工]