色谱

色谱 ›› 2018, Vol. 36 ›› Issue (11): 1140-1146.DOI: 10.3724/SP.J.1123.2018.07013

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱同时测定植物油中14种营养成分

彭祖茂, 朱丽, 邓梦雅, 张协光, 郑裕辉   

  1. 深圳市计量质量检测研究院, 国家营养食品质量监督检验中心(广东), 广东 深圳 518109
  • 收稿日期:2018-07-12 出版日期:2018-11-08 发布日期:2014-09-30
  • 通讯作者: 朱丽.Tel:(0755)27528545,E-mail:foodtestzl@126.com.
  • 基金资助:

    广西高校中青-教师基础能力提升项目（2017KY1382）.

Simultaneous determination of 14 nutrients in vegetable oils by ultra high performance liquid chromatography-tandem mass spectrometry

PENG Zumao, ZHU Li, DENG Mengya, ZHANG Xieguang, ZHENG Yuhui   

  1. Shenzhen Academy of Metrology and Quality Inspection, National Nutrition Food Testing Center(Guangdong), Shenzhen 518109, China
  • Received:2018-07-12 Online:2018-11-08 Published:2014-09-30
  • Supported by:

    Project of Improving the Basic Ability of Young and Middle-aged Scholars in Guangxi Colleges (No. 2017KY1382).

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摘要：

建立超高效液相色谱-串联质谱同时检测植物油中4种生育酚、4种生育三烯酚、4种植物甾醇、β-胡萝卜素和角鲨烯等14种营养成分的方法。样品经皂化处理后，采用石油醚提取浓缩，用甲醇定容。采用Poroshell 120 PFP色谱柱（150 mm×3.0 mm，2.7 μm）分离，以0.1%（v/v）甲酸水溶液和0.1%（v/v）甲酸甲醇溶液为流动相进行梯度洗脱，流速为0.3 mL/min。采用大气压化学电离源、正离子模式，在选择反应监测模式下扫描。结果表明，14种营养成分在0.05~10.0 mg/L范围内相关系数≥0.9971；在不同添加水平下，14种营养成分的回收率为80.7%~100.5%，相对标准偏差＜6.0%（n=6）；方法的检出限和定量限分别为0.01~0.30 μg/g和0.04~1.00 μg/g。该法灵敏、准确，分析时间快，稳定性好，适用于植物油中14种营养成分的同时检测。

关键词: -胡萝卜素, &beta, 超高效液相色谱-串联质谱, 角鲨烯, 维生素E, 植物油, 植物甾醇

Abstract:

A method for the simultaneous determination of four tocopherols, four tocotrienols, four phytosterols, β-carotene and squalene by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. After saponification, the samples were extracted with petroleum ether, and the extract solution was concentrated by rotary evaporation. The residue was dried under a N2 atmosphere and dissolved with methanol. The 14 nutrients were separated on a Poroshell 120 PFP column (150 mm×3.0 mm, 2.7 μm) by gradient elution with 0.1% (v/v) formic acid aqueous solution and methanol containing 0.1%(v/v) formic acid as the mobile phases at a flow rate of 0.3 mL/min. The detection was performed using an atmospheric pressure chemical ionization (APCI)-mass spectrometer with selective reaction monitoring (SRM) in positive mode. The results were linear in the range of 0.05-10.0 mg/L for the 14 nutrients, and the correlation coefficients (r) were no less than 0.9971. The average recoveries of the 14 nutrients in the vegetable oil samples ranged from 80.7% to 100.5% at three spiked levels, and the relative standard deviations (RSDs) were less than 6.0%. The limits of detection (LODs) ranged from 0.01 to 0.30 μg/g. The limits of quantification (LOQs) were in the range of 0.04-1.00 μg/g. The proposed method is sensitive, accurate, fast and stable, and is suitable for the simultaneous determination of the 14 nutrients in vegetable oil samples.

Key words: β-carotene, phytosterols, squalene, ultra high performance liquid chromatography-mass spectrometry (UHPLC-MS/MS), vegetable oil, vitamin E

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