| Targeting at the mycotoxins in food matrix and combining with the current tendency and concern of food safety,this research was developed in three aspects: 1)the development of detection method for patulin in food matrix;2)the establishment of detection method for sterigmatocystin in food matrix;and 3)the improvement of detection methods for multiple mycotoxins in soybean.A method has been developed for the determination of patulin in fruit products by high performance liquid chromatography tandem mass spectrometry.The clear juice was directly purified and enriched by ProElut PXA.Besides,the cloud juice,solid-liquid and solid samples were primarily hydrolyzed by pectinase,extracted by ethyl acetate,concentrated,redissolved by acetic acid solution(pH=4.0),and purified and enriched by ProElut PXA.The chromatographic separation was performed on a Waters HSS T3(2.1 mm×100 mm,1.8 μm)column bygradient elution with acetonitrile and water.The patulin was detected by mass spectrometry(MS)coupled with electrospray negative ionization(ESI)in the mode of multiple reaction monitoring(MRM).Accurate determination was achieved using isotope as internal standard.It was proved to be a practical method which could completely satisfy the standard requirement GB 2761-2011 of patulin detection.In conclusion,this method was reliable,accurate and sensitive,and could be used for the analysis of patulin in fruit products.We developed a method for the determination of sterigmatocystin in plant food by performance liquid chromatography tandem mass spectrometry.Samples was extracted by mixed solution,purified and enriched by HLB,removed grease by PRIME HLB,then was separated by reversed phase column.The sterigmatocystin was detected by MS with electrospray positive ionization in the mode of multiple reaction monitoring(MRM).Accurate determination was achieved by using isotope as internal standard.The good linearity was observed.This method was reliable,accurate and sensitive,and could be used for the analysis of sterigmatocystin in plant food,such as wheat,maise,peanut and soybean.This study established a detection method of 33 kinds of mycotoxins in soybean by UPLC-MS/MS.As the complex matrix-soybean has high phosphatide and protein content,the method firstly optimized theextraction condition,including the proportion of organic phase and the acidic condition.Then,adopt dispersive solid-phase extraction method to purify,screening 10 kids of dSPE filer and select the suitable adsorbent.Finally,to establish a method for 33 kinds of mycotoxins and validate the methodology,inspect linear range,LOQ,accuracy and precision.In this study,the established detection methods of patulin,sterigmatocystin and a variety of mycotoxins in food matrix were highly sensitive,accurate and reliable for the requirement of daily monitoring and provided the technical supports for food security. |