食品科学 ›› 2021, Vol. 42 ›› Issue (14): 187-194.doi: 10.7506/spkx1002-6630-20210217-186

• 成分分析 • 上一篇    下一篇

GC-MS和LC-MS/MS分析麦粉中烷基间苯二酚同系物组成

黄沁沁,樊凤娇,李彭,樊艳,邹燕羽,方勇   

  1. (南京财经大学食品科学与工程学院,江苏 南京 210023)
  • 发布日期:2021-07-27
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2016YFD0401203); 全国粮食行业青年拔尖人才服务行业需求自主选题项目(LQ2018301);江苏高校优势学科建设工程资助项目(PAPD)

Analysis of Alkylresorcinol Homologues in Wheat Flour by GC-MS and LC-MS/MS

HUANG Qinqin, FAN Fengjiao, LI Peng, FAN Yan, ZOU Yanyu, FANG Yong   

  1. (College of Food Science and Engineering, Nanjing University of Finance and Economics, Nanjing 210023, China)
  • Published:2021-07-27

摘要: 建立气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)联用法和液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)法测定麦粉中烷基间苯二酚组成。样品经乙酸乙酯超声提取,在GC-MS中,硅烷化衍生处理,采用选择离子监测模式进行测定,以外标法进行定量;在LC-MS/MS中,经固相萃取富集净化,以C18色谱柱分离,采用电喷雾负离子模式扫描、多反应监测模式检测,以外标法进行定量。结果表明,GC-MS和LC-MS/MS均在0.001~5 μg/mL质量浓度范围内有良好的线性关系(R2>0.98),GC-MS法的检出限为2.0~6.1 μg/g,加标回收率在94.17%~99.15%之间,相对标准偏差(relative standard deviation,RSD)在2.94%~4.87%之间;LC-MS/MS法的检出限为2.0~8.4 μg/g,加标回收率在89.05%~99.06%之间,RSD在2.21%~4.17%之间。本研究建立了2 种线性关系良好、低检测限、高灵敏度的检测方法,均可适用于市售麦粉产品中烷基间苯二酚同系物定性定量分析,将为麦类全谷物产品品质控制与检测提供技术指导。

关键词: 烷基间苯二酚;麦粉品质;气相色谱-质谱联用法;液相色谱-串联质谱法;超声提取;净化

Abstract: In this study, two methods were established for the determination of the content and homologue composition of alkylresorcinols (ARs) in wheat flour, namely gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The sample was ultrasonically extracted with ethyl acetate. The extract was derivatized by silanization before GC-MS analysis in the selected ion monitoring (SIM) mode. Quantification was performed the by external standard method. Before LC-MS/MS, the extract was enriched and purified by solid phase extraction (SPE) on a C18 chromatographic column, and the separated analytes were detected in the negative ion scanning mode using multiple reaction monitoring (MRM) and quantified similarly by the external standard method. The results showed that both methods exhibited a good linear relationship in the concentration range of 0.001–5 μg/mL. The detection limit of the GC-MS method was 2.0–6.1 μg/g, and the spiked recoveries were 94.17%–99.15%, with relative standard deviation (RSD) of 2.94%–4.87%. The detection limit of the LC-MS/MS method was 2.0–8.4 μg/g, and the spiked recoveries were 89.05%–99.06%, with RSD of 2.21%–4.17%. These two detection methods, thanks to their good liner relationship, low detection limit, and high sensitivity, could be suitable for the qualitative and quantitative analysis of AR homologues in commercially available wheat flour products, which will provide a technical reference for the quality control and detection of whole-grain wheat products.

Key words: alkylresorcinols; wheat flour quality; gas chromatography-mass spectrometry; liquid chromatography-tandem mass spectrometry; ultrasonic extraction; purification

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