色谱

色谱 ›› 2017, Vol. 35 ›› Issue (9): 949-956.DOI: 10.3724/SP.J.1123.2017.05001

• 研究论文 • 上一篇    下一篇

超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱快速测定大米中15种营养成分

朱丽1, 谭微2, 彭祖茂1, 邓梦雅1, 张协光1, 杨国武1   

  1. 1. 深圳市计量质量检测研究院, 广东 深圳 518109;
    2. 广西科技大学鹿山学院食品与化学工程系, 广西 柳州 545616
  • 收稿日期:2017-05-04 出版日期:2017-09-08 发布日期:2017-09-15
  • 通讯作者: 朱丽,Tel:(0755)27528545,E-mail:foodtestzl@126.com.
  • 基金资助:

    广东省质量技术监督局科技项目（2017CZ12）.

Rapid determination of 15 nutrients in rice by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry

ZHU Li1, TAN Wei2, PENG Zumao1, DENG Mengya1, ZHANG Xieguang1, YANG Guowu1   

  1. 1. Shenzhen Academy of Metrology and Quality Inspection, Shenzhen 518109, China;
    2. Department of Food and Chemical Engineering, Lushan College of Guangxi University of Science and Technology, Liuzhou 545616, China
  • Received:2017-05-04 Online:2017-09-08 Published:2017-09-15
  • Supported by:

    Administration of Quality and Technology Supervision of Guangdong Province Project (No. 2017CZ12).

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138

被引次数

2

摘要：

建立了超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱（UHPLC-LTQ/Orbitrap HRMS）同时快速检测大米中15种营养成分（8种维生素E、6种 γ-谷维素及 β-胡萝卜素）的方法。样品经过含0.05%（v/v） 2，6-二叔丁基-4-甲基苯酚（BHT）的甲醇溶液超声提取处理后，用Poroshell 120 PFP色谱柱（150 mm×3.0 mm， 2.7 μm）分离，以0.1%（v/v）甲酸水溶液和含0.1%（v/v）甲酸的甲醇溶液为流动相，在正离子模式下通过UHPLC-LTQ/Orbitrap HRMS进行全扫描分析。15种营养成分可在13 min内获得满意的分离效果。15种营养成分在各自的线性范围内线性关系良好，相关系数（r） ≥ 0.9950， 15种营养成分的检出限（S/N=3）为0.2~1.8 μg/L，定量限（S/N=10）为0.7~6.1 μg/L，在3个添加水平下的平均加标回收率分别为73.2%~101.5%，相对标准偏差（RSD）为1.1%~5.0% （n=3）。该法准确，高效，可靠，适用于大米中多种营养成分的同时测定。

关键词: -谷维素, -胡萝卜素, &beta, &gamma, 超高效液相色谱, 大米, 维生素E, 线性离子阱/静电场轨道阱高分辨质谱, 营养成分

Abstract:

A rapid method was developed for the simultaneous determination of 15 nutrients containing eight vitamin E, six γ-oryzanols and β-carotene in rice by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UHPLC-LTQ/Orbitrap HRMS). The analytes were extracted by methanol containing 0.05% (v/v) 2,6-di-tert-butyl-4-methylphenol (BHT) under the ultrasonic condition, then separated by a Poroshell 120 PFP column (150 mm×3.0 mm, 2.7 μm) with a gradient elution program using 0.1% (v/v) formic acid aqueous solution and methanol containing 0.1% (v/v) formic acid as mobile phases. The detection was performed using an LTQ/Orbitrap HRMS detector with full scan in positive ion mode. Fifteen nutrients were simultaneously separated within 13 min. Furthermore, matrix effects of the white and brown rices were investigated. The correlation coefficients (r) were ≥ 0.9950 in the linear ranges of the 15 nutrients. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) of the 15 nutrients were 0.2-1.8 μg/L and 0.7-6.1 μg/L, respectively. At the three spiked levels, the recoveries were 73.2%-101.5% with the relative standard deviations (RSDs) ranging from 1.1% to 5.0% (n=3). The method is accurate, efficient and reliable. It is suitable for the simultaneous determination of various nutrients in rice.

Key words: β-carotene, γ-oryzanol, linear ion trap-orbitrap high resolution mass spectrometer (LTQ/Orbitrap HRMS), nutrients, rice, ultra high performance liquid chromatography (UHPLC), vitamin E

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