Citation: JIANG Li-Yan, ZHAO Qi-Yang, GONG Lei, LIU Yan-Yu, ZHANG Yao-Hai, MA Liang, JIAO Bi-Ning. Rapid Determination of Five Alternaria Mycotoxins in Citrus by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2015, 43(12): 1851-1858. doi: 10.11895/j.issn.0253-3820.150370 shu

Rapid Determination of Five Alternaria Mycotoxins in Citrus by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

JIANG Li-Yan ^1,2 ,
ZHAO Qi-Yang ^2,4 ,
GONG Lei ^2,4 ,
LIU Yan-Yu ^2,4 ,
ZHANG Yao-Hai ^2,4 ,
MA Liang ^1,2,, ,
JIAO Bi-Ning ^1,2,3,4,,

1.
¹ College of Food Science, Southwest University, Chongqing 400715, China;

Corresponding author: MA Liang, JIAO Bi-Ning,
Received Date: 5 May 2015
Available Online: 22 July 2015
Fund Project: 本文系国家重点基础研究发展计划(973计划)项目(No.2013CB127803) (973计划)项目(No.2013CB127803)国家自然科学基金项目(No.31301476) (No.31301476)农业部现代农业(柑桔)产业技术体系建设专项(CARS-27) (柑桔)产业技术体系建设专项(CARS-27)2015年国家农产品质量安全风险评估重大专项(GJFP2015004) (GJFP2015004)中央高校基本科研业务费专项(XDJK2013B035)资助项目。 (XDJK2013B035)

A novel method was developed for the rapid determination of five alternaria mycotoxins, alternariol, alternariol monomethyl ether, altenuene, tentoxin and tenuazonic acid, in citrus using ultra-high performance liquid chromatography-tandem mass spectrometry. The sample was prepared using the modified QuEChERS(quick, easy, cheap, effective, rigged, and safe) method to complete the extraction and clean-up steps in one procedure. In this QuEChERS method, sample was extracted with acetonitrile(1.5% formic acid), then salted out with anhydrous MgSO4 and NaCl, separated on an ACQUITY UPLC BEH C₁₈ with gradient elution by using acetonitrile and 0.1% formic acid aqueous as eluant, and detected by UPLC-MS/MS under negative(ESI⁺) electrospray ionization and MRM models. Under these conditions, five alternaria mycotoxins made a good linearity in the concentration range of 2.0-100μg/L with R²>0.9922, and the limits of detection of the instrument were in the range of 0.11-0.91μg/kg. Three spiked levels of five altenaria mycotoxins at 5, 20 and 100μg/kg were investigated, and the recoveries ranged from 71% to 112% with the relative standard deviations(RSDs) varying from 1.1% to 9.9%, which met the requirement of mycotoxins determination.
- Altenaria mycotoxins,
- Ultra-high performance liquid chromatography-tandem mass spectrometry,
- Citrius,
- QuEChERS method
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