Grains In The Rapid Screening Of Multiple Mycotoxin Residues In Confirmatory Detection Method

A class of secondary metabolites produced by the filamentous fungal metabolites is called mycotoxins, plant by these mycotoxins cause serious economic damage to humans. Currently known types are hundreds of mycotoxins, which structurally diverse variety of physical and chemical properties. Part of mycotoxins can make people carcinogenic, teratogenic and mutagenic effects occur. To avoid contamination of food by fungal toxins and harm to human health, food quality and the need to strengthen safety supervision. Development of multi-component detection of mycotoxins is especially important.In this study, aflatoxin（B₁, B₂, G₁, G₂）, T-2 toxin, ochratoxin nine kinds of mycotoxins, has developed a quick and easy, targeted, high-sensitivity performance liquid chromatography- tandem mass spectrometry（UPLC-MS / MS） method to complete the multi-component detection of mycotoxins, the accuracy of the test results. Include the following:1. Establish multi mycotoxins in cereals QuEChERS pre-treatment methods. Each pretreatment conditions were optimized, including the amount of acetic acid, the volume of extract, selection cleaning agent. Final in 1% acetic acid- acetonitrile（v / v1: 3） extract, no cleaning agent conditions for improved treatment conditions QuEChERS before.2.By optimizing ultra HPLC mobile phase gradient elution and MS conditions for the establishment of the eight kinds of mycotoxins ultra performance liquid chromatography- tandem mass spectrometry detection（UPLC-MS / MS） are. UPLC using Phenomenex Kinetex 2.6u XB C18（100 mm × 4.6 mm, 2.6μm） column with a mobile phase containing 0.1% formic acid + 5mM ammonium acetate in water, and 0.5% acetic acid + 5mM ammonium acetate methanol. MS（ESI） ion source ion source, MRM monitored. The limit of detection 0.5-2000μg / kg, the linear correlation coefficient R2≥0.9990, a good linear relationship. The average recovery of 60% to 100%, and the relative standard deviation（RSD） 2.0% 11.40%. The intra- and inter-day precision ranges from 2% to 9% and 12% to 17%. This method is suitable for rapid screening of mycotoxins analysis and confirmed positive samples.3.Establishment of DON in cereals in the solid phase extraction method. Compare HLB cartridges and Supel Tox DON small column purification process, similar to HLB cartridges come with Supel Tox DON cartridge cleaning effect, taking into account the cost problem is detected, the eventual adoption of HLB solid phase extraction column. By optimizing performance liquid chromatography with gradient elution and MS conditions, ultra performance liquid chromatography DON toxin- tandem mass spectrometry detection（UPLC-MS / MS） are. The method detection limit of 20 1000μg / kg, the linear correlation coefficient R2 = 0.9976, a good linear relationship. The average recovery rate is the average recovery was 85.6% 82%, RSD less than 10%. The detection limit is 20μg / kg, the limit of quantification is 50μg / kg.