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

引用本文: 范志辰, 韩铮, 郭文博, 赵志辉. 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[J]. 色谱, 2017, 35(6): 627-633. doi: 10.3724/SP.J.1123.2017.02010 shu

Citation: FAN Zhichen, HAN Zheng, GUO Wenbo, ZHAO Zhihui. Simultaneous determination of 30 mycotoxins in different feed products by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(6): 627-633. doi: 10.3724/SP.J.1123.2017.02010 shu

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

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
基金项目:
沪农科攻字（2014）第3-2号（G20140302）.

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:

English

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

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 Date: 12 February 2017
Fund Project:
Shanghai Agriculture Applied Technology Development Program of China (No. G20140302).

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:

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

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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

English

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

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通讯作者: 陈斌, bchen63@163.com

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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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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