食品科学 ›› 2018, Vol. 39 ›› Issue (18): 292-301.doi: 10.7506/spkx1002-6630-201818045

• 安全检测 • 上一篇    下一篇

固相萃取柱净化-超高效液相色谱-串联质谱法快速测定液态乳中14 种真菌毒素

孙晓冬,郝杰,毛婷,邵瑞婷,姜洁*   

  1. (北京市食品安全监控和风险评估中心,北京 100094)
  • 出版日期:2018-09-25 发布日期:2018-09-18
  • 基金资助:
    国家重点研发计划“国家质量基础的共性技术研究与应用”专项(2016YFF0203802); 北京市科技计划项目(Z161100000616007)

Determination of 14 Mycotoxins in Liquid Milk by Solid-Phase Extraction Coupled with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

SUN Xiaodong, HAO Jie, MAO Ting, SHAO Ruiting, JIANG Jie*   

  1. (Beijing Municipal Center for Food Safety Monitoring and Risk Assessment, Beijing 100094, China)
  • Online:2018-09-25 Published:2018-09-18

摘要: 建立使用固相萃取柱净化液态乳中14 种真菌毒素(黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B1、伏马毒素B2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸)多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取,固相萃取柱Oasis PRiME HLB净化后,以0.1%甲酸溶液与乙腈为流动相,经ACQUITY UPLC HSS T3色谱柱(2.1?mm×100?mm,1.8?μm)分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明:14?种真菌毒素的定量限(RSN≥10)为0.5~5?μg/kg,高、中、低3?个添加水平时,平均回收率为67.7%~112.7%,相对标准偏差为0.43%~7.28%。该方法的检测速度快,净化效果较好,基质干扰较少,灵敏度高,结果准确、可靠,可用于液态乳中真菌毒素的检测分析。

关键词: 液态乳, 固相萃取柱, 超高效液相色谱-串联质谱, 真菌毒素, 快速

Abstract: A rapid method was established for detecting 14 mycotoxins (aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, aflatoxin M1, ochratoxin A, citrinin, T-2 toxin, sterigmatocystin, fumonisin B1, fumonisin B2, zearalenone, deoxynivalenol, and penicillic acid) in liquid milk by solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were defatted and extracted with 0.1% formic acid acetonitrile and the extract was cleaned up with Oasis PRiME HLB solid-phase extraction column. The analytes were separated on HSS T3 column (2.1 mm × 100 mm, 1.8 μm) with a mobile phase composed of 0.1% formic acid and acetonitrile using gradient elution. Detection was carried out by tandem mass spectrometry using positive ionization in the multiple-reaction monitoring (MRM) mode. An external standard method was applied for quantification. Results showed that the limits of quantitation (LOQs) of 14 mycotoxins in matrices were between 0.5 and 5 μg/kg. Average recoveries at 3 different spiked levels were 67.7%–112.7% with relative standard deviation (RSD) of 0.43%–7.28%. With the advantages of rapidity, high purification efficiency, low matrix interference and accurate and reliable results, the method is useful for the analysis of mycotoxins in liquid milk.

Key words: liquid milk, solid-phase extraction column, ultra-performance liquid chromatography-tandem mass spectrometry, mycotoxins, rapid detection

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