Determination Method Of Zearalenone By Means Of High-performance Liquid Chromatography

Background and objective:Zearalenone(ZEA)is a secondary fungal metabolite produced by several species of Fusarium in corn,wheat,grain growth process,mainly by Fusarium graminearum and Fusarium culmorum.ZEA takes on serious gential and growth toxicity.ZEA has caused serious harm to human and animals with heavy toxicity,a wide range of contamination,and the difficulties of removal,so it has serious impact on crop yield and has lowered the quality of agricultural products and feed,has aroused great concern to the majority of researchers,so food and agriculture organization and world health organization has to resolve the issue as a urgent matter.Chinese in the main category of cereal,as the same time,china is also a grain trade great power,so establishment of ZEA simple and fast,sensitive and effective detection method in food,to protect the health of Chinese and grain trade have positive economy significance.Research methods:1.Using acetonitrile-water,Acetonitrile-NaCl solution by ultrasonic extraction of ZEA,after filtration,take methanol-water,Acetonitrile-methanol-water as mobile phase,fluorescence detection,high-performance liquid chromatography detection ZEA,establishment of ZEA fast detection method of high-performance liquid chromatography in corn.2.Using Acetonitrile-NaCl solution by ultrasonic extraction,rotary evaporation vacuum concentration,the purification of solid phase extraction,fluorescence detection,high-performance liquid chromatography detection ZEA in corn.ZEA extractioned process focused on discussion solid-liquid ratio,Acetonitrile-NaCl solution,NaCl concentration and ultrasonic extraction time on extraction effect. Purification condition focused on research solid phase extraction column activation, solvent the sample composition and the proportion,solvents pass solid-phase extraction column purification effext.chromatographic condtions discussion of selection column,detector,detection wavelength,mobile phase to detection results effect.Conclusion:1.Sample extraction by acetonitrile-water(9:1 V/V),Agilent XDB C₁₈column separation,using methanol-water(7:3 V/V)as moblie phase,detection of ZEA indexes are as follows,standard curve linear regression equation of ZEA is Y=361.25X-1154.20,R²=0.9997,linear range is 20～1×10⁴ng/ml.Added standard is 120μg/kg of corn samples recovery is 87.0～96.4%,within-day and inter-day Relative standard deviation was 5.8%,4.0%.The detection limit was 10μg/kg based on a signal-to-noise ratio of 3:1.2.Sample extraction by Acetonitrile-40g/L NaCl solution(8:2 V/V),Agilent XDB C₁₈column separation,using Acetonitrile-methanol-water(46:8:46 V/V)as moblie phase,detection of ZEA indexes are as follows,standard curve linear regression equation of ZEA is Y=625.27X-2666.8,R～2=0.9998,linear range is 20～1×104ng/ml.Added standard is 60,120,240μg/kg of corn samples recovery is 81.8～97.1%,within-day and inter-day Relative standard deviation range was 1.9-4.4%,The detection limit was 10μg/kg based on a signal-to-noise ratio of 3:1.3.Sample extraction by Acetonitrile-40g/L NaCl solution(8:2 V/V),the purification of solid phase extraction,Agilent XDB C₁₈column separation,using methanol-water(65:35 V/V)as moblie phase,detection of ZEA indexes are as follows,standard curve linear regression equation of ZEA is Y=442.91X+878.65, R2=0.9998,linear range is 20～1×104ng/ml.Added standard is 60,120,240μg/kg of corn samples recovery is 78.2%⁸9.6%,within-day and inter-day Relative standard deviation range was 1.5%～3.9%,The detection limit was 10μg/kg based on a signal-to-noise ratio of 3:1.Using Acetonitrile-methanol-water(46:8:46 V/V) as moblie phase,Added standard is 60,120,240μg/kg of corn samples recovery is 78.5%～88.5%,within-day and inter-day Relative standard deviation range was 2.3%～4.1%,The detection limit was 10μg/kg based on a signal-to-noise ratio of 3:1.This paper focused on discussion a variety of ZEA extraction,purification, concentration condition.Single study methanol-water,Acetonitrile-methanol-water as mobile phase to detection results effect.To ZEA provide sensitive,reliable and practical detection analysis methods.