超高效合相色谱-质谱法快速分离测定4种单脂肪酸甘油酯  

Rapid Separation and Determination of Four Fatty Acid Monoglycerides by Ultra Performance Convergence Chromatography-Mass Spectrometry

作　　者：林春花[1] 芮培欣[1] 雷志伟[1] 严楠[1] 许招会[2] 廖维林[1] 

机构地区：[1]江西师范大学国家单糖化学合成工程技术研究中心,南昌330027 [2]江西师范大学化学化工学院,南昌330027

出　　处：《应用化学》2016年第2期238-244,共7页Chinese Journal of Applied Chemistry

基　　金：国家科技支撑计划(No.2012BAE07B00)资助项目~~

摘　　要：采用超高效合相色谱-质谱(UPC^2-MS)技术,建立了一种快速分离植物油单脂肪酸甘油酯中单软脂酸甘油酯、单硬脂酸甘油酯、单油酸甘油酯和单亚油酸甘油酯4种单甘酯的测定方法。以葵花籽油为原料,通过脂肪酶催化甘油解反应制备单甘酯。样品用正己烷/异丙醇(体积比7∶3)溶解,采用超临界CO2-甲醇/乙腈(体积比1∶1)梯度洗脱,经ACQUITY UPC2BEH^2-EP(100 mm×2.1 mm,1.7μm)色谱柱分离,通过质谱检测器在正离子电喷雾模式下对目标化合物进行分析,外标法定量。结果表明,4种单甘酯化合物在线性范围内线性关系良好,线性相关系数(R^2)均大于0.9983;目标物的检出限(S/N≥3)为0.036~0.093 mg/L;3个加标水平下的回收率在88.50%~110.00%之间,相对标准偏差为1.01%~4.04%。本方法具有检出限低、分析速度快、分离效果好、分析成本低等优点,为脂肪酸酯类物质的分离测定提供了新的色谱技术平台。A method for rapid separation and determination of four fatty acid monoglycerides,via ultraperformance convergence chromatography-mass spectrometry,was developed. Fatty acid monoglycerides were prepared by lipase-catalyzed glycerolysis using sunflower oil as the starting material. The main monoglycerides are monopalmitin,monostearin,monoolein,and monolinolein. The samples were dissolved by n-hexane /isopropanol（ 7∶ 3 volume ratio）,separated in 6 min on the column of ACQUITY UPC^2 BEH 2-EP（ 100 mm ×2. 1 mm,1. 7 μm） with gradient elution of carbon dioxide and methanol / acetonitrile（ 1 ∶ 1 volume ratio）system,and then detected by MS detector in the ESI^＋mode. The results verified that the standard curves for the four components were obtained with good correlation coefficients（ R^2）〉 0. 9983 in their concentration ranges. The limits of detection（ LOD,S / N = 3） for the four monoglycerides are in the range of 0. 036 -0. 093 mg / L. The recoveries for the four monoglycerides at three spiked levels（ low,middle,high） are88. 50% - 110. 00% with the relative standard deviations of 1. 01% - 4. 04%. The proposed UPC^2-MS method is featured with low detection limit,less time consuming,good separation and low cost. It would provide a new chromatographic technology platform for the detection of fatty acid esters.

关 键 词：超高效合相色谱-质谱法 单脂肪酸甘油酯 甘油解 葵花籽油 

分 类 号：O657.6[理学—分析化学]