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中国精品科技期刊2020
陈悦铭,黄景初,徐婷,等. 多功能免疫亲和柱净化-超高效液相色谱串联质谱法快速检测咖啡豆中的11种真菌毒素[J]. 食品工业科技,2021,42(16):285−293. doi: 10.13386/j.issn1002-0306.2020110294.
引用本文: 陈悦铭,黄景初,徐婷,等. 多功能免疫亲和柱净化-超高效液相色谱串联质谱法快速检测咖啡豆中的11种真菌毒素[J]. 食品工业科技,2021,42(16):285−293. doi: 10.13386/j.issn1002-0306.2020110294.
CHEN Yueming, HUANG Jingchu, XU Ting, et al. Rapid Determination of 11 Mycotoxins in Coffee Bean through Multifunctional Purification and Immunoaffinity Column Coupled to High-performance Liquid Chromatography Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(16): 285−293. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020110294.
Citation: CHEN Yueming, HUANG Jingchu, XU Ting, et al. Rapid Determination of 11 Mycotoxins in Coffee Bean through Multifunctional Purification and Immunoaffinity Column Coupled to High-performance Liquid Chromatography Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(16): 285−293. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020110294.

多功能免疫亲和柱净化-超高效液相色谱串联质谱法快速检测咖啡豆中的11种真菌毒素

Rapid Determination of 11 Mycotoxins in Coffee Bean through Multifunctional Purification and Immunoaffinity Column Coupled to High-performance Liquid Chromatography Tandem Mass Spectrometry

  • 摘要: 建立了同时测定咖啡豆中11种真菌毒素的超高效液相色谱-串联质谱分析方法,实验考察了色谱柱选择、提取溶剂组成、固相萃取柱选择、流动相比例对分析结果的影响。以咖啡豆为研究对象,样品均质后,经乙腈-水-甲酸(85+14+1,V/V)振荡提取,离心,过Oasis PRiME HLB柱,取净化液10 mL用磷酸缓冲液稀释至50 mL,经多功能免疫亲和柱净化,氮吹、50%乙腈复溶,以0.1%甲酸-2 mmol/L乙酸铵溶液-乙腈为流动相,用Waters BEH C18柱分离,超高效液相色谱-质谱仪分析,内标法定量。结果表明,11种真菌毒素在各自线性范围内线性关系良好,相关系数均大于0.998,检出限为0.008~0.544 μg/kg。在低、中、高3个添加水平下的平均回收率为80.2%~114%,相对标准偏差为1.4%~7.9%。本方法步骤简便、快速高效,适用于咖啡豆中11种真菌毒素的同时测定分析。

     

    Abstract: A method was established for the simultaneous determination of 11 fungal toxins in coffee beans by ultra-performance liquid chromatography tandem mass spectrometry, the effects of column selection, extracting solvent composition, solid phase extraction column selection and flow phase ratio on the analysis results were examined. Taking coffee beans as the research object, the samples were extracted by acetylene-water-formic acid (85+14+1, V/V) purified by Oasis PRiME HLB, the purification diluted with phosphoric acid buffer, nitrogen blowing after the purified by multi-functional immunoaffinity column, determined by ultra-performance liquid chromatography tandem mass spectrometry after resoluble with 50% acetylene, with 0.1% foric acid-2 mmol/L ammonium acetate solution-acetylene as the flow phase, separated by Waters BEH C18 column, determined by ultra-performance liquid chromatography tandem mass spectrometry quantitated by internal standard method. The results showed that, the linear correlation of 11 mycotoxins were greater than 0.998, the limits of detection were in the range of 0.008~0.544 μg/kg. The average recoveries at the three spiked levels were 80.2%~114% with relative standard deviations of 1.4%~7.9%. This method was simple, fast and efficient, and would be suitable for the co-measurement and analysis of 11 mycotoxins in coffee beans.

     

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