Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Alternaria Toxins in Grapes

Wenbo Guo; Kai Fan; Dongxia Nie; Jiajia Meng; Qingwen Huang; Junhua Yang; Yuanyuan Shen; Emmanuel K Tangni; Zhihui Zhao; Yongjiang Wu; Zheng Han

doi:10.3390/toxins11020087

Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Alternaria Toxins in Grapes

Toxins (Basel). 2019 Feb 1;11(2):87. doi: 10.3390/toxins11020087.

Authors

Wenbo Guo¹, Kai Fan², Dongxia Nie³, Jiajia Meng⁴, Qingwen Huang^{5

6}, Junhua Yang⁷, Yuanyuan Shen⁸, Emmanuel K Tangni⁹, Zhihui Zhao¹⁰, Yongjiang Wu¹¹, Zheng Han¹²

Affiliations

¹ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. guowenbo@saas.sh.cn.
² Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. fankai1983@gmail.com.
³ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. niedongxia@saas.sh.cn.
⁴ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. mengjiajia@saas.sh.cn.
⁵ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. huangqingwen@zju.edu.cn.
⁶ College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China;. huangqingwen@zju.edu.cn.
⁷ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. yangjunhua@saas.sh.cn.
⁸ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. shenyuanyuan@saas.sh.cn.
⁹ Organic Contaminants and Additives, Sciensano, Tervuren 3080, Belgium. emmanuel.tangni@sciensano.be.
¹⁰ Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. zhao9912@hotmail.com.
¹¹ College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China;. yjwu@zju.edu.cn.
¹² Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China. hanzheng@saas.sh.cn.

Abstract

A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography⁻tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six Alternaria toxins. After validation by determining the linearity (R² > 0.99), recovery (77.8⁻101.6%), sensitivity (limit of detection in the range of 0.03⁻0.21 μg kg^-1, and limit of quantification in the range of 0.09⁻0.48 μg kg^-1), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of Alternaria toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with Alternaria toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10⁻1.64 μg kg^-1, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the Alternaria toxins contamination in grapes in China.

Keywords: Alternaria toxins; UHPLC-MS/MS; grape; modified QuEChERS.

Publication types

Research Support, Non-U.S. Gov't

MeSH terms

Alternaria*
Biological Monitoring
China
Chromatography, High Pressure Liquid
Food Contamination / analysis*
Mycotoxins / analysis*
Tandem Mass Spectrometry
Vitis / chemistry*

Substances

Mycotoxins