食品科学

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SPE-GC-GC-TOFMS检测油脂中游离甾醇及精炼废弃油脂的判别

徐宝成1,2,3,张良晓2,4,王 华5,*,杨青青2,6,罗登林3,李培武2,4,6,7,8,*   

  1. 1.西北农林科技大学食品科学与工程学院,陕西 杨凌 712100;2.中国农业科学院油料作物研究所,湖北 武汉 430062;
    3.河南科技大学食品与生物工程学院,河南 洛阳 471003;4.农业部油料及制品质量监督检验测试中心,
    湖北 武汉 430062;5.西北农林科技大学葡萄酒学院,陕西葡萄与葡萄酒工程技术中心,陕西 杨凌 712100;
    6.农业部油料产品质量安全风险评估实验室,湖北 武汉 430062;7.农业部油料作物生物学重点实验室,
    湖北 武汉 430062;8.农业部生物毒素检测重点实验室,湖北 武汉 430062
  • 出版日期:2015-01-25 发布日期:2015-01-16
  • 通讯作者: 王 华,李培武WANG Hua5
  • 基金资助:

    “十二五”国家科技支撑计划项目(2012BAK08B03);“双打”相关产品检验鉴定方法研究专项(2012104010-4);
    国家自然科学基金青年科学基金项目(21205118)

A Method for Determination of Free Phytosterols Derived from Vegetable Oils by SPE-GC-GC-TOFMS and Its Application for Discrimination of Refined Waste Oils

XU Baocheng1,2,3, ZHANG Liangxiao2,4, ,*, YANG Qingqing2,6, LUO Denglin3, LI Peiwu2,4,6,7,8,*   

  1. 1. College of Food Science and Engineering, Northwest A&F University, Yangling 712100, China;
    2. Oil Crops Research Institute of the Chinese Academy of Agricultural Sciences, Wuhan 430062, China;
    3. College of Food and Bioengineering, Henan University of Science and Technology, Luoyang 471003, China;
    4. Quality Inspection and Test Center for Oilseeds Products, Ministry of Agriculture, Wuhan 430062, China;
    5. Shanxi Engineering Research Center for Viti-Viniculture, College of Enology, Northwest A&F University, Yangling 712100, China;
    6. Laboratory of Risk Assessment for Oilseeds Products, Ministry of Agriculture, Wuhan 430062, China;
    7. Key Laboratory of Biology and Genetic Improvement of Oil Crops, Minstry of Agriculture, Wuhan 430062, China;
    8. Key Laboratory of Detection for Mycotoxins, Ministry of Agriculture, Wuhan 430062, China
  • Online:2015-01-25 Published:2015-01-16
  • Contact: WANG Hua,LI Peiwu

摘要:

研究开发一种基于固相萃取的植物油中游离甾醇的快速分离及多维气相色谱串联飞行时间质谱检测方法。与普通一维气相色谱相比,14 种游离甾醇及β-香树脂醇的三甲基硅烷化衍生物在多维气相色谱上得到了更好地分离,并且检测灵敏度更高。方法学验证结果表明:胆固醇、菜籽甾醇、芸薹甾醇和β-谷甾醇的检出限分别为0.03、0.04、0.04 mg/100 g油和0.05 mg/100 g油,定量限分别为0.06、0.08、0.08 mg/100 g油和0.08 mg/100 g油,在不同添加水平条件下的加标回收率皆高于93%,相对标准偏差在1.4%~10.0%之间。同时,利用本方法对6 种商品植物油及25 份精炼废弃油脂中的游离甾醇进行检测,并分析其在植物油和废弃油脂中的分布模式,提出了以判别指数对废弃油脂进行鉴别的方法,结果显示25 份精炼废弃油脂被完全正确识别。

关键词: 多维气相色谱-飞行时间质谱, 固相萃取, 游离甾醇, 精炼废弃油脂, 判别

Abstract:

In this study, a multidimensional gas chromatography coupled to time-of-flight mass spectrometry (GCGC-
TOFMS) method was established to determine free sterols in edible oils extracted by rapid solid-phase extraction.
Compared with conventional one-dimensional gas chromatography, a better separation and a higher detection sensitivity
for trimethylsilyl derivatives of free sterols and β-amyrin were obtained by GC-GC. Meanwhile, the validation results of
the established method indicated that the limits of detection for cholesterol, brassicasterol, campesterol and β -sitosterol
were 0.03, 0.04, 0.04 and 0.05 mg/100 g of oil, respectively; and the limits of quantification for the four sterols were
0.06, 0.08, 0.08 and 0.08 mg/100 g of oil, respectively. In addition, the recovery rates of the selected four sterols spiked at
three different levels were higher than 93% with a relative standard deviation ranging from 1.4% to 10.0%. Based on the
established method, six types of edible oils and 25 refined waste oils were analyzed by GC-GC-TOFMS, and the distribution
mode of free sterols in normal vegetable oils and waste oils were also analyzed. Moreover, a method based on discrimination
index (DI) was proposed to identify refined waste oils, and the results indicated that the refined waste oils could be
discriminated from the normal six edible oils completely.

Key words: multidimensional gas chromatography-time-of-flight-mass spectrometry (GC-GC-TOFMS), solid phase extraction (SPE), free phytosterols, refined wasted oils, discrimination

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