食品科学 ›› 2010, Vol. 31 ›› Issue (24): 385-388.doi: 10.7506/spkx1002-6630-201024084

• 分析检测 • 上一篇    下一篇

液相色谱串联质谱检测食品中的黄曲霉毒素

郑 燕,王远兴* ,李瑾瑾   

  1. 1. 南昌大学 食品科学与技术国家重点实验室
  • 收稿日期:2010-06-29 出版日期:2010-12-25 发布日期:2010-12-29
  • 通讯作者: 王远兴 E-mail:yuanxingwang@ncu.edu.cn
  • 基金资助:

    食品科学与技术国家重点实验室自由探索资助课题(SKLF-TS-200915);国家自然科学基金项目(21045006)

Determination of Aflatoxins in Food by Liquid Chromatography-Tandem Mass Spectrometry

ZHENG Yan,WANG Yuan-xing*,LI Jin-jin   

  1. State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047, China
  • Received:2010-06-29 Online:2010-12-25 Published:2010-12-29
  • Contact: WANG Yuan-xing E-mail:yuanxingwang@ncu.edu.cn

摘要:

为提高黄曲霉毒素的检测灵敏度,建立快速液相色谱串联质谱(LC-MS/MS)法对食品中的4 种黄曲霉毒素B1、B2、G1、G2 进行定性定量分析。样品粉碎后用体积比为84:16 的乙腈- 水混合液提取,过滤后通过真菌毒素净化柱进样,采用C18 柱分离,0.1% 甲酸溶液和甲醇做流动相,以60:40 比例等度洗脱,质谱在多反应监测(MRM)的正离子模式下进行分析。4 种组分在5min 内完全分离,而且此方法线性关系良好,黄曲霉毒素B1、B2、G1、G2 的检出限分别是0.012、0.009、0.013、0.007μg/kg,平均加标回收率在80%~95% 之间,相对标准偏差小于5%。该方法快速灵敏、准确可靠,其检出限可满足欧盟地区严格的黄曲霉毒素限量标准。

关键词: 液相色谱串联质谱, 黄曲霉毒素, 食品

Abstract:

In order to improve detection sensitivity of aflatoxions, a liquid chromatography-tandem mass spectrometry method was established for the simultaneously qualitative and quantitative analysis of aflatoxins B1, B2, G1 and G2. Samples were sequentially extracted by acetonitrile-water at a ratio of 84:16 (V/V), cleaned up with multifunctional cleaning column. After injection, the chromatographic separation was achieved on a C18 column using a mobile phase composed of a mixture of 0.1% formic acid and methanol through gradient elution. The analysis was realized by multiple reaction-monitoring modes. Under above conditions, aflatoxins B1, B2, G1 and G2 could be completely separated in 5 min with an excellent linear relationship. The determination limits for 4 kinds of aflatoxins were 0.012, 0.009, 0.013μg/kg and 0.007μg/kg, respectively. The recovery rate of spiked samples was in the range of 80%-95% with a relative standard deviation less than 5%. This method can provide a rapid, sensitive, accurate and reproducible detection for aflatoxins and its detection limit is sensitive enough to meet the European regulation for aflatoxins.

Key words: liquid chromatography-tandem mass spectrometry, aflatoxins, food

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