Multiclass Mycotoxin Analysis In Wine And Its Raw Materials By Ultra High Performance Liquid Chromatography–tandem Mass Spectrometry Using A Procedure Based On QuEChERS

Rcently,with the increase in domestic consumption of wine,the developed countries and developing countries more and more followed with interest on these metabolites,due to its effect on human health and domestic and foreign trade.It can be seen that was imperative to research on mycotoxin contamination in wine.The number of high performance liquid chromatography–tandem mass spectrometry(LC–MS/MS)methods reported for multiclass analysis of mycotoxins in food has increased considerably due to the high selectivity and sensitivity reached,and also because of the compatibility of sample extract and analyte physicochemical characteristics with the mobile phases and ionization sources employed in LC–MS/MS.In general the extraction of mycotoxins from liquid samples is based on solid phase extraction(SPE)using immunoaffinity columns or other type of sorbents.Meanwhile,other extraction techniques such as liquid–liquid extraction(LLE),solid phase microextraction(SPME)and liquid phase microextraction(LPME)have also been applied.In recent years,QuEChERS method with the advantages of experimental steps less,simple operation,and high purification efficiency on complex sample,its application on mycotoxin detection was increasingly widespread.The aim of this study was to develop an analytical method for the simultaneous determination of aflatoxins B1,B2,G1,G2,M1,ochratoxin A and B,zearalenone,deoxynivalenol,neosolaniol,HT-2 toxin,T-2 toxin,diacetoxyscirpenol,fumonisin B1,sterigmatocystine,citrinin,mycophenolic acid,cyclopiazonic acid,penicillic acid and mevinolin in Vitis vinifera and wine using ultra high performance liquid chromatography–tandem mass spectrometry(UHPLC-MS/MS).The developed methodology was applied to the analysis of 78 samples at Hexi Corridor.The results show that:1.The wine/water ratio was 5:5,1 g sodium chloride and 4 g anhydrous magnesium sulfate was selected as salt addition,omitting the dSPE purification step,then,direct drying by anhydrous magnesium sulfate after for detection using UHPLC-MS/MS(ESI positive mode),obtain the best extraction efficiency;2.In a wide linear range,obtaining instrument limits of detection(0.06~10 μg/L)lower than those usually permitted by legislation in food matrices,with precisions lower than 10%,R2≥0.9963.The recoveries was observed at the concentration of 2.5 μg/L,5 μg/L and 10 μg/L,were 85.61%~117.82%,RSD between 5.95% and 17.49%.3.The validated methodology has been first applied to the analysis of 36 Vitis vinifera samples and 42 wine samples from Jiayuguan,Zhangye and Wuwei of Hexi Corridor.The results shown that PCA,FB1,MPA,ZEN and CPA were detected in the Vitis vinifera,the content of MPA was up to 81.26 μg/L.In wine,in addition to the most commonly found OTA,there are some lower occurrence frequency of mycotoxins were detected,such as AFB2,CPA and ZEN,the content of MPA in wine was lower than in Vitis vinifera,but the detection frequency up to 48%.4.It was remarkable that in none of the samples the concentration of mycotoxins exceed the maximum levels established by Regulation 1881/2006/EC and their subsequent amendments.