15-羟基十五烷酸合成环十五内酯体系定量分析方法比较  

Comparison of Quantitative Analysis Methods for Synthesis of Cyclopentadecanolide from 15-Hydroxypentadecanoic Acid

作　　者：程海军 孙泽宇 赖芳[1] 李伟光[1] 马丽[1] 刘雄民[1] CHENG Haijun;SUN Zeyu;LAI Fang;LI Weiguang;MA Li;LIU Xiongmin(School of Chemistry and Chemical Engineering,Guangxi University,Nanning 530004,China)

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《食品科技》2020年第5期293-298,共6页Food Science and Technology

基　　金：国家自然科学基金项目(21502027);广西自然科学基金项目(2015GXNSFAA139041);广西大学科研基金项目(XBZ130010);广西大学“大学生创新创业训练计划”项目(201910593193)。

摘　　要：为探寻合适的15-羟基十五烷酸合成环十五内酯反应体系定量分析方法,采用液相色谱法、气相色谱非衍生化法和衍生化法分别对样品中15-羟基十五烷酸和环十五内酯进行分析。结果表明:液相色谱法15-羟基十五烷酸保留时间为6.21 min,环十五内酯保留时间为16.32 min,但在样品中的色谱峰不明显。采用SH-Stabilwax-DA酸性专用色谱柱(30 m×0.25 mm,0.25μm)的气相色谱检测15-羟基十五烷酸,非衍生化法和衍生化法的RSD值分别为1.36%~2.23%和2.17%~3.44%。利用非衍生化法同时测定15-羟基十五烷酸和环十五内酯,RSD值分别为1.36%~2.23%、2.18%~3.48%。非衍生化法无需经过复杂的衍生化直接进样,可对15-羟基十五烷酸和环十五内酯同时分析,操作简便。The suitable quantitative analysis method for the cyclopentadecanolide synthesis reaction with 15-hydroxypentadecanoic acid was explored.The 15-hydroxypentadecanoic acid and cyclopentadecanolide in the samples were analyzed by liquid chromatography,non-derivatization and derivatization of gas chromatography respectively.The results showed that the retention time of 15-hydroxypentadecanoic acid and cyclopentadecanolide was 6.21 min and 16.32 min respectively by liquid chromatography,but their chromatographic peaks were not obvious in the samples.15-hydroxypentadecanoic acid was detected by gas chromatography using a SH-Stabilwax-DA acidic column(30 m×0.25 mm,0.25μm).The relative standard deviation(RSD)values of the non-derivatization method and the derivatization method were 1.36%~2.23%and 2.17%~3.44%,respectively.The RSD values of 15-hydroxypentadecanoic acid and cyclohexaolactone were detected simultaneously by the nonderivatization method were 1.36%~2.23%and 2.18%~3.48%,respectively.The non-derivatization method could inject directly without complicated derivatization.It can analyze 15-hydroxypentadecananoic acid and cyclopentadecanone simultaneously,and the operation is simple and convenient.

关 键 词：15-羟基十五烷酸 环十五内酯 定量分析 非衍生化法 直接进样 

分 类 号：O657.63[理学—分析化学]