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高效液相色谱-串联质谱法同时测定饲料中11种霉菌毒素

魏云计 冯民 朱臻怡 何健 沈金荣 何正和 秦娴 周利英

色谱2017,Vol.35Issue(8):891-896,6.
色谱2017,Vol.35Issue(8):891-896,6.DOI:10.3724/SP.J.1123.2017.03042

高效液相色谱-串联质谱法同时测定饲料中11种霉菌毒素

Simultaneous determination of 11 mycotoxins in feeds by high performance liquid chromatography-tandem mass spectrometry

魏云计 1冯民 1朱臻怡 1何健 1沈金荣 1何正和 1秦娴 1周利英2

作者信息

  • 1. 淮安出入境检验检疫局国家饲料安全检测重点实验室(淮安), 江苏 淮安 223001
  • 2. 昆山出入境检验检疫局, 江苏 昆山 215300
  • 折叠

摘要

Abstract

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 11 mycotoxins in feeds.The samples were extracted with acetonitrile, then cleaned up by multifunctional purification column filler and PRIME HLB solid phase extraction column.The 11 mycotoxins were separated on an Agilent Zorbax SB-C18 column (150 mm×2.1 mm, 3.5 μm) with gradient elution program, and methanol-5 mmol/L ammonium acetate solution containing 0.1%(v/v) formic acid were used as mobile phases.The target compounds were detected under electrospray ionization (ESI) both in positive and negative modes with multiple reaction monitoring mode, and quantified by internal standard method.The results indicated that the 11 mycotoxins showed good linear relationships in their respective linear ranges, and the correlation coefficients were greater than 0.99.The limits of quantification (LOQs) were between 2.0 and 50.0 μg/kg.The average recoveries were between 79.3% and 101.6% at three spiked levels (1, 2 and 5 times LOQs) with relative standard deviations (RSDs) of 5.9%-13.2% (n=5).The method is simple, rapid, sensitive, and can be used for the analysis of the 11 mycotoxins in feeds.

关键词

高效液相色谱-串联质谱/固相萃取/多功能净化柱填料/霉菌毒素/饲料

Key words

high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)/solid phase extraction (SPE)/multifunctional purification column filler/mycotoxins/feeds

分类

化学化工

引用本文复制引用

魏云计,冯民,朱臻怡,何健,沈金荣,何正和,秦娴,周利英..高效液相色谱-串联质谱法同时测定饲料中11种霉菌毒素[J].色谱,2017,35(8):891-896,6.

基金项目

江苏检验检疫局科研项目(2016KJ35).Jiangsu Entry-Exit Inspection and Quarantine Bureau Science and Technology Project (No.2016KJ35). (2016KJ35)

色谱

OA北大核心CSCDCSTPCDMEDLINE

1000-8713

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