Residues’ Detection And Naturally Contaminated Sample’s Development Of Sudan Dyes In Egg Products

Abuse of Sudan dyes in food are common,Sudan standard sample plays a very important role for quality control and residues’ detection of Sudan. This study regards Sudan dyes(Sudan Ⅰ, Sudan Ⅱ, SudanⅢ and SudanⅣ) in egg products as main research subject,establishes and optimizes high performance liquid chromatography-mass spectrometry method of Sudan dyes in egg products,and uses Deuterated Sudan as Isotopic internal standard for quantitative.The main contents and conclusions of this research are as follows:(1) The pretreatment method of Sudan dyes in egg products has established. The final sample pretreatment conditions were:using hexane as extraction agent and using 15minutes as ultrasonic extraction time. The optimum conditions of solid phase extraction was:using Sudan dedicated SPE column as the solid phase extraction column, using dichloromethane as elution solvent and using 5mL as elute volume.(2) The high performance liquid chromatography-mass spectrometric method of Sudan dye residual quantity in egg products has established. The linear range of Sudan Ⅰ～Ⅳ was 0～50μ/kg, the detection limits in eggs were 0.20,0.24,0.20,0.31 μ/kg, the detection limits in preserved eggs were 0.26,0.20,0.12,0.14 μg/kg, the detection limits in salted eggs were 0.21,0,25,0.21,0.25 μg/kg. All the correlation coefficient were larger than 0.999. By adding 1～10μ/kg Sudan mixed standard solution to eggs, preserved eggs and salted eggs using this method for recovery test, the average recovery rate of Sudan Ⅰ was 84.6～104.2%, the precision of Sudan Ⅰ was 4.4～10.5%; the average recovery rate of SudanⅡ was 80.9～102.7%, the precision of Sudan Ⅱ was 4.8～0.9%; the average recovery rate of SudanⅢ 83.2～103.2%, the precision of Sudan Ⅲ was 4.6～10.4%;the average recovery Sudan Ⅳ was 80～ 101.5%, the precision of Sudan IV was 4.2～0.3%. the standard deviation was 2.0～10.9%. The experiment proved that the method was simple, high accuracy and sensitivity, meanwhile, all the detection limit were less than 1.0μg/kg. all these characteristics of this method proved that it is suitable for detecting Sudan dyes in eggs.(3) Feeding chickens with food containing prohibited pigment -Sudan dye. the eggs containing trace of Sudan were abtained. The conducted regular on residues’ degradation of Sudan dye in eggs were preliminary investigation, which did prepare for preparing and uniformity tests of naturally contaminated samples of residues of Sudan dye.