高效液相色谱-串联质谱法同时测定饲料中11种霉菌毒素

doi:10.3724/SP.J.1123.2017.03042

色谱 ›› 2017, Vol. 35 ›› Issue (8): 891-896.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

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

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

收稿日期:2017-03-30 出版日期:2017-08-08 发布日期:2013-11-25
通讯作者: 魏云计,Tel:83336508,E-mail:jswyj_84@163.com
基金资助:
江苏检验检疫局科研项目（2016KJ35）.

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

WEI Yunji¹, FENG Min¹, ZHU Zhenyi¹, HE Jian¹, SHEN Jinrong¹, HE Zhenghe¹, QIN Xian¹, ZHOU Liying²

1. State Key Laboratory of Feed Safety Testing(Huai'an), Huai'an Entry-Exit Inspection and Quarantine Bureau, Huai'an 223001, China;
2. Kunshan Entry-Exit Inspection and Quarantine Bureau, Kunshan 215300, China

Received:2017-03-30 Online:2017-08-08 Published:2013-11-25
Supported by:
Jiangsu Entry-Exit Inspection and Quarantine Bureau Science and Technology Project (No. 2016KJ35).

摘要/Abstract

摘要：

建立了高效液相色谱-串联质谱（HPLC-MS/MS）同时检测饲料中11种霉菌毒素的分析方法。样品经乙腈提取，MycoSep 228多功能净化柱填料和PRIME HLB固相萃取柱净化；采用Agilent Zorbax SB-C18色谱柱（150 mm×2.1 mm，3.5 μ m）分离，以甲醇和5 mmol/L乙酸铵水溶液（含0.1%（v/v）甲酸）为流动相梯度洗脱；采用ESI源正、负离子同时扫描，多反应监测（MRM）模式测定，内标法定量。结果表明，11种目标物在各自的线性范围内线性关系良好，相关系数均大于0.99，定量限为2.0~50.0 μ g/kg。11种霉菌毒素在3个加标水平（1、2、5倍定量限）下的平均回收率为79.3%~101.6%，相对标准偏差（RSD）为5.9%~13.2%（n=5）。该法简单快速，净化效果好，灵敏度高，适用于饲料中11种霉菌毒素的分析。

关键词: 多功能净化柱填料, 高效液相色谱-串联质谱, 固相萃取, 霉菌毒素, 饲料

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 μ m) 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 μ g/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.

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

中图分类号:

O658

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.

WEI Yunji, FENG Min, ZHU Zhenyi, HE Jian, SHEN Jinrong, HE Zhenghe, QIN Xian, ZHOU Liying. Simultaneous determination of 11 mycotoxins in feeds by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(8): 891-896.

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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

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

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