1. 江西师范大学化工研究开发中心
2. 国家单糖化学合成工程技术研究中心
3. 华东交通大学基础学院化学化工系
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林春花, 严楠, 许招会, 等. 超高效合相色谱-质谱法快速检测植物油脂中5种脂肪酸含量[J]. 分析测试学报, 2014,33(11):1322-1326.
Rapid Detection of Five Fatty Acids in Vegetable Oils Based on Ultra Performance Convergence Chromatography-Mass Spectrometry[J]. 2014,33(11):1322-1326.
建立了一种超高效合相色谱-质谱(UPC2 -MS)技术快速检测植物油脂中棕榈酸、硬脂酸、油酸、亚油酸、亚麻酸5种常见脂肪酸的方法。样品用正己烷溶解后,采用超临界CO2-甲醇/乙腈(体积比,1∶1)梯度洗脱,经ACQUITY UPC2 BEH 2-EP(2.1 mm i.d.×100 mm,1.7 μm)色谱柱分离,通过质谱检测器对目标化合物进行分析,外标法定量。结果表明,5种脂肪酸在0.5~100 mg/L范围内具有良好线性(相关系数不小于0.998 5);在3个加标水平下,样品的回收率为90.5%~105.4%,相对标准偏差为0.8%~2.9%;方法的检出限(S/N≥3)为0.07~0.26 mg/L。相比于其他方法,本方法简单快速,分离效果好,且无需对脂肪酸样品进行衍生化,为UPC2技术在油脂相关分析领域的进一步应用和研究提供了参考。
A rapid method was developed for the detection of 5 common fatty acids,including palmitic acid,stearic acid,oleic acid,linoleic acid and linolenic acid,in vegetable oils based on ultra-performance convergence chromatography-mass spectrometry(UPC2-MS).The sample was dissolved with n hexane,followed by clean up of extract using 022 μm organic phase filter.The fatty acids were separated in 3 min on a column of ACQUITY UPC2 BEH 2-EP(2.1 mm i.d.×100 mm,1.7 μm) by gradient elution with carbon dioxide and methanol-acetonitrile(by volume,1∶1) system,and finally detected by MS detector.The results showed that the calibration curves of five analytes were linear in the range of 0.5-100 mg/L with correlation coefficients(r2) not less than 0.998 5.The recoveries for five fatty acids at three spiked levels were in the range of 90.5%-105.4% with relative standard deviations of 0.8%-2.9%.The limits of detection for the target compounds in the method ranged from 0.07 mg/L to 0.26 mg/L.In comparison with other methods,this method was simple,rapid,and had good separation effect.Furthermore,the method could provide reference for further research and application of UPC2 technology in oil related analysis field without derivatization of fatty acid samples.
超高效合相色谱-质谱法植物油脂未衍生化脂肪酸
ultra-performance convergence chromatography-mass spectrometry(UPC2-MS)vegetable oilsunderivatizationfatty acids
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