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

doi:10.11944/j.issn.1000-0518.2016.02.150188

摘要/Abstract

摘要：

采用超高效合相色谱-质谱(UPC²-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,1.7 μm)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(R²)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。

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

Abstract:

A method for rapid separation and determination of four fatty acid monoglycerides, via ultra-performance 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 UPC² 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(R²)>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) are 88.50%~110.00% with the relative standard deviations of 1.01%~4.04%. The proposed UPC²-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.

Key words: ultra-performance convergence chromatography-mass spectrometry(UPC2-MS), fatty acid monoglyceride, glycerolysis, sunflower oil

林春花, 芮培欣, 雷志伟, 严楠, 许招会, 廖维林. 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[J]. 应用化学, 2016, 33(2): 238-244.

LIN Chunhua, RUI Peixin, LEI Zhiwei, YAN Nan, XU Zhaohui, LIAO Weilin. Rapid Separation and Determination of Four Fatty Acid Monoglycerides by Ultra Performance Convergence Chromatography-Mass Spectrometry[J]. Chinese Journal of Applied Chemistry, 2016, 33(2): 238-244.

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