色谱

色谱 ›› 2017, Vol. 35 ›› Issue (6): 627-633.DOI: 10.3724/SP.J.1123.2017.02010

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定不同饲料中30种真菌毒素

范志辰1, 韩铮2, 郭文博2, 赵志辉2   

  1. 1. 上海海洋大学食品学院, 上海 201306;
    2. 上海市农业科学院农产品质量标准与检测技术研究所, 上海 201403
  • 收稿日期:2017-02-12 出版日期:2017-06-08 发布日期:2013-09-29
  • 通讯作者: 赵志辉,Tel:(021)52235463,E-mail:zhao9912@hotmail.com.
  • 基金资助:

    沪农科攻字（2014）第3-2号（G20140302）.

Simultaneous determination of 30 mycotoxins in different feed products by ultra high performance liquid chromatography-tandem mass spectrometry

FAN Zhichen1, HAN Zheng2, GUO Wenbo2, ZHAO Zhihui2   

  1. 1. College of Food Science & Technology, Shanghai Ocean University, Shanghai 201306, China;
    2. Institute for Agro- Food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China
  • Received:2017-02-12 Online:2017-06-08 Published:2013-09-29
  • Supported by:

    Shanghai Agriculture Applied Technology Development Program of China (No. G20140302).

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被引次数

1

摘要：

采用QuEChERS前处理技术，建立了超高效液相色谱-串联质谱（UHPLC-MS/MS）检测不同饲料样品（预混料、浓缩料和配合料）中30种真菌毒素含量的分析方法。饲料样品经5 mL水和5 mL含1%（v/v）甲酸的乙腈溶液提取后，取上清液氮吹至近干，残渣经1 mL 5 mmol/L醋酸铵水溶液-乙腈（80：20，v/v）复溶后，上机测定。采用基质匹配标准曲线结合同位素内标法进行定量分析。在低、中、高3个添加水平下，30种真菌毒素的平均加标回收率为72.0%~118.4%（n=5），30种真菌毒素在各自的线性范围内线性关系良好，相关系数（r2）≥0.99，检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.7~20 μg/L和2~50 μg/L。该法简单、快速、实用性强，适用于预混料、浓缩料和配合料中30种真菌毒素的定量分析。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 饲料, 真菌毒素

Abstract:

A method for the simultaneous determination of 30 mycotoxins in different feed products was developed using a QuEChERS pretreatment procedure coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The samples were extracted with 5 mL water and 5 mL acetonitrile containing 1% (v/v) formic acid. An aliquot of the supernatant was dried by nitrogen gas, re-dissolved by 1mL water containing 5 mmol/L ammonium acetate-acetonitrile (80:20, v/v), and analyzed by UHPLC-MS/MS. Matrix-matched calibration curves and internal standards were used for accurate quantification. Satisfactory recoveries at low, medium and high spiked levels were ranged from 72.0% to 118.4% (n=5). Good linear relationships were obtained, the correlation coefficients (r2) were greater than 0.99. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) ranged from 0.7 μg/L to 20 μg/L and from 2 μg/L to 50 μg/L, respectively. The proposed method is simple, rapid and valuable, which can be a powerful tool for quantitative analysis of the 30 mycotoxins in premixed feed, concentrated feed and formula feed products.

Key words: feed, mycotoxins, QuEChERS, ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)

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