单甘酯硅烷化衍生及气相色谱-质谱分析  

Silylation Derivatization of Monoglyceride and Analysis by Gas Chromatography-Mass Spectrometry

作　　者：楼乔明[1,2] 李哲 刘连亮[1] 张进杰[1] 杨文鸽[1] 薛长湖[2] LOU Qiaoming;LI Zhe;LIU Lianliang;ZHANG Jinjie;YANG Wenge;XUE Changhu(College of Food and Pharmaceutical Sciences,Ningbo University,Ningbo,Zhejiang 315800;College of Food Science and Engineering,Ocean University of China,Qingdao,Shandong 266003)

机构地区：[1]宁波大学食品与药学学院,浙江宁波315800 [2]中国海洋大学食品科学与工程学院,山东青岛266003

出　　处：《核农学报》2020年第11期2519-2525,共7页Journal of Nuclear Agricultural Sciences

基　　金：“水产”浙江省重中之重学科开放基金项目(xkzsc1531);浙江省自然科学基金项目(LQ15C200002)。

摘　　要：为分析罗氏海盘车性腺的单甘酯组成,本研究对单甘酯的衍生方法和色谱条件进行优化,并对单甘酯硅烷化衍生物的断裂规律和质谱特征进行分析,同时对罗氏海盘车性腺的单甘酯组成进行分析测定。结果表明,三甲基硅烷化法对单甘酯具有理想的衍生效果,且通过弱极性毛细管柱HP-5MS(30 m×0.25 mm×0.25μm)对单甘酯硅烷化衍生物取得了理想的色谱分离效果。根据断裂规律和质谱特征,1-单甘酯硅烷化衍生物的特征离子为m/z 73、m/z 205、[M-103]^+(基峰离子)和[M-15]^+;2-单甘酯硅烷化衍生物的特征离子为m/z 73(基峰离子)、m/z 129、m/z 218、[M+H-162]^+和[M-15]^+。单甘酯硅烷化衍生物的色谱保留时间具有一定的规律性,其中2-单甘酯衍生物先于1-单甘酯衍生物出峰。同时,从罗氏海盘车中共鉴定出8种单甘酯,以1-单软脂酸甘油酯(1-C16:0-MG)和1-单硬脂酸甘油酯(1-C18:0-MG)等1-单甘酯为主,而2-单甘酯含量较低。本研究结果为单甘酯的衍生、色谱分析和质谱鉴定提供了一定的理论参考。In order to analyze the monoglyceride compositions of Asterias rollestoni gonad,the derivative methods and chromatographic conditions of monoglycerides were optimized,and the fragmentation rules and mass spectrometry characteristics of monoglyceride derivatives were analyzed and monoglyceride compositions in Asterias rollestoni gonad were also detected in this paper.The results indicated that trimethylsilylation had ideal derivative effects on monoglycerides,and the ideal chromatographic separation effects of monoglyceride derivatives were obtained by the weak-polar glass capillary column(HP-5 MS,30 m×0.25 mm×0.25μm).Moreover,the characteristic ions of 1-monoglyceride derivatives were m/z 73,m/z 205,[M-103]^+(base-peak ion)and[M-15]^+,while 2-monoglyceride derivatives were m/z 73(base-peak ion),m/z 129,m/z 218,[M+H-162]^+and[M-15]^+.Gas chromatographic retention time of monoglyceride derivatives displayed certain regularitys,and 2-monoglyceride derivatives were eluted earlier than 1-monoglyceride derivatives.Additionally,eight monoglycerides were identified from Asterias rollestoni gonad,which were mainly consisted of 1-monopalmitin(1-C16:0-MG)and 1-monostearin(1-C18:0-MG),while the contents of 2-monoglycerides were relatively low.This research provides theoretical references for derivatization,chromatographic analysis and mass spectrometric identification of monoglycerides.

关 键 词：单甘酯 衍生方法 质谱特征 气相色谱-质谱法(GC-MS) 罗氏海盘车 

分 类 号：O657.63[理学—分析化学] TQ423.2[理学—化学]