色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 397-402.DOI: 10.3724/SP.J.1123.2014.12004

• 研究论文 • 上一篇    下一篇

超高效合相色谱-质谱法快速分析食用植物油中常见脂肪酸

林春花, 谢贤清, 范乃立, 涂媛鸿, 陈彦, 廖维林   

  1. 江西师范大学, 国家单糖化学合成工程技术研究中心, 江西 南昌 330027
  • 收稿日期:2014-12-02 修回日期:2015-01-08 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 廖维林
  • 基金资助:

    国家科技支撑计划课题(2014BAE13B02,2012BAE07B00).

Fast analysis of common fatty acids in edible vegetable oils by ultra-performance convergence chromatography-mass spectrometry

LIN Chunhua, XIE Xianqing, FAN Naili, TU Yuanhong, CHEN Yan, LIAO Weilin   

  1. National Research Center of Monosaccharide Chemical Synthesis Engineering, Jiangxi Normal University, Nanchang 330027, China
  • Received:2014-12-02 Revised:2015-01-08 Online:2015-04-08 Published:2015-03-30

PDF

351

被引次数

15

摘要：

建立了超高效合相色谱-质谱(UPC2-MS)快速分析6种食用植物油(玉米油、葵花籽油、大豆油、茶油、菜籽油、花生油)中棕榈酸、硬脂酸、油酸、亚油酸、亚麻酸等5种常见脂肪酸的方法,并比较了这6种食用油中上述5种脂肪酸的含量差异。采用皂化反应对植物油进行前处理,以ACQUITY UPC2 BEH 2-EP色谱柱(100 mm×2.1 mm, 1.7 μm)为分析柱,以超临界CO2-甲醇/乙腈(1:1, v/v)为流动相进行梯度洗脱,流速为0.8 mL/min。在电喷雾负离子模式下进行检测,外标法定量。结果表明:5种脂肪酸标准物质在0.5~100 mg/L范围内呈现良好的线性关系,相关系数为0.9985~0.9998,定量限(S/N≥10)为0.15~0.50 mg/L;在3个添加水平下,样品的加标回收率为89.61%~108.50%;方法重复性的相对标准偏差(RSD)为0.69%~3.01%。该方法简单、快速、分离效果好,无需对脂肪酸样品进行衍生化,已成功地用于玉米油、葵花籽油、橄榄油、茶油、大豆油和花生油等6种食用油中常见脂肪酸含量的测定。

关键词: 超高效合相色谱-质谱法, 食用植物油, 未衍生化, 脂肪酸

Abstract:

A fast analytical method for five common fatty acids in six edible vegetable oils was developed by ultra-performance convergence chromatography-mass spectrometry (UPC2-MS). The five fatty acids are palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid. Their contents in the corn oil, sunflower oil, soybean oil, tea oil, rapeseed oil and peanut oil were compared. The chromatographic separation was performed on an ACQUITY UPC2 BEH 2-EP column (100 mm×2.1 mm, 1.7 μm) using the mobile phases of carbon dioxide and methanol/acetonitrile (1:1, v/v) with gradient elution. The separated compounds were detected by negative electrospray ionization ESI--MS. The results showed that the reasonable linearities were achieved for all the analytes over the range of 0.5-100 mg/L with the correlation coefficients (R2) of 0.9985-0.9998. The limits of quantification(S/N≥10)of the five fatty acids were 0.15-0.50 mg/L. The recoveries of the five fatty acids at three spiked levels were in the range of 89.61%-108.50% with relative standard deviations of 0.69%-3.01%. The developed method showed high performance, good resolution and fast analysis for the underivatized fatty acids. It has been successfully used to detect the five fatty acids from corn oil, sunflower oil, soybean oil, tea oil, rapeseed oil and peanut oil.

Key words: edible vegetable oils, fatty acids, ultra-performance convergence chromatography-mass spectrometry(UPC2-MS), underivatization

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