超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的9种真菌毒素

doi:10.7506/spkx1002-6630-201020075

食品科学 ›› 2010, Vol. 31 ›› Issue (20): 360-366.doi: 10.7506/spkx1002-6630-201020075

超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的9种真菌毒素

廉慧锋¹，赵笑天²，王蓉珍³，宋欢¹，林勤保^{2 ,*}

1.山西出入境检验检疫局技术中心
2.山西大学应用化学研究所
3.山西省分析测试中心

收稿日期:2010-06-22 出版日期:2010-10-25 发布日期:2010-12-29
通讯作者: 林勤保 E-mail:qblin@sxu.edu.cn
基金资助:
山西省科技攻关计划项目(20100311067)

Simultaneous Determination of 9 Kinds of Mycotoxins in Maize, Peanut and Wheat by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

LIAN Hui-feng1，ZHAO Xiao-tian2，WANG Rong-zhen3，SONG Huan1，LIN Qin-bao2,*

1. Shanxi Entry-exit Inspection and Quarantine Bureau, Taiyuan 030024, China ；
2. Institute of Applied Chemistry, Shanxi University, Taiyuan 030006, China ；
3. Shanxi Analyse and Test Center, Taiyuan 030006, China

Received:2010-06-22 Online:2010-10-25 Published:2010-12-29
Contact: LIN Qin-bao2,* E-mail:qblin@sxu.edu.cn

摘要/Abstract

摘要：

建立玉米、花生、麦仁中9 种真菌毒素的超高效液相色谱- 串联质谱确证方法。样品用甲醇- 水溶液和磷酸缓冲液(PBS)双重提取后直接过真菌毒素免疫亲和柱净化；氮气吹干后用的乙腈- 水溶液(50:50，V/V)定容，超高效液相色谱- 串联质谱(LC-MS-MS)测定，电喷雾正、负离子(ESI+、ESI －)多反应模式监测。结果表明，样品中真菌毒素在0.1～400μg/kg 范围内时与其峰面积呈良好线性关系，定量限为0.1～20μg/kg，3 个加标水平下平均回收率为59.5%～118.8%，相对标准偏差为2.4%～12.8%，符合痕量分析的要求。

关键词: 超高效液相色谱-串联质谱, 真菌毒素, 玉米, 花生, 麦仁

Abstract:

A simultaneous determination method for nine kinds of mycotoxins in maize, peanut and wheat was developed using ultra-high performance liquid chromatography-tendem mass spectrometry (UPLC-MS/MS). Samples were sequentially extracted with PBS solution followed by 70% methanol, and then the extracts were pooled and cleaned up with immunoaffinity column, followed by blowing to dryness under nitrogen gas stream, reconstitution with acetonitrile/water mixture before the analysis on UPLC-MS/MS. The MS conditions used were negative (ESI+) and positive (ESI－) electrospray ionization and MRM models. The results indicated as follows: 1) all the nine kinds of mycotoxins had good linear relationship with peak area over the range from 0.1 to 400μg/kg, and the detection limits for them ranged from 0.1 to 20μg/kg; and 2) The average recovery rates in the above three matrices spike at three levels were between 59.5% and 118.8%, with a relative standard deviation (RSD) varying from 2.4% to 12.8%. This analytical method meets the requirements for trace assays. In addition, it is simple, rapid, accurate and suitable for the simultaneous determination of nine kinds of mycotoxins in maize, peanut and wheat.

Key words: UPLC-MS/MS, mycotoxin, maize, peanut, wheat

中图分类号:

TS201.6

廉慧锋1，赵笑天2，王蓉珍3，宋欢1，林勤保2,*. 超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的9种真菌毒素[J]. 食品科学, 2010, 31(20): 360-366.

LIAN Hui-feng1，ZHAO Xiao-tian2，WANG Rong-zhen3，SONG Huan1，LIN Qin-bao2,*. Simultaneous Determination of 9 Kinds of Mycotoxins in Maize, Peanut and Wheat by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2010, 31(20): 360-366.

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超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的9种真菌毒素

Simultaneous Determination of 9 Kinds of Mycotoxins in Maize, Peanut and Wheat by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

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