Analysis Of Sulfonamides Residues In Animal Derived Food

The use of antibiotic drugs is prevalent in animal breeding, sulfonamides are widely used toprevent and treat disease of animal derived from food. With the public's increasing concern withthe food safety, residues of antibiotic drugs in animal derived food should arouse regards. Themisuse of antibiotic drugs in animal breeding can cause residues in animal derived food, theseresidues can influence human food security and pollute environment possibly. Therefore, it isnecessary to establish the analysis method for the detection of sulfonamides residues in animal foodproducts. The main research area in this thesis can be included as follows:1. The method of GB/T 4789.27-2003 was employed to evaluate the practicability of themicrobiological method that was used to analysis of sulfonamides residues in milk. This methodwas simple, easy to operate and not requiring expensive apparatus or equipments. Whiletime-consuming, unquantitative were it's shortage; The most important was that the sensitivity ofthis method was very low, the detection limit was higher than maximum residue limitation ofsulfonamide residues in milk and the method was poor in practicability.2. established the extraction and corresponding analytical method of six sulfonamides inanimal tissue, the extracting solvent was dichloromethane and the sample was extracted byaccelerated solvent extraction (ASE), ultrasonic-assistant extraction and homogenization extractionrespectively, and cleaned up with n-hexane, separated on a HPLC reversed column (C₁₈ column)and diode array detector (DAD) detection, external standard method was quantitative analyticalmethod.For accelerated solvent extraction, as index for the added recovery of sulfonamides, variousextracting parameters were investigated to optimize the extracting conditions that affected therecovery of sulfonamides during ASE, the suitable conditions of ASE were as follows: theoperating pressure was 500 psi, the temperature was 40℃, the static extracting time was 5 min andthree cycles.The sample treatment were accelerated solvent extraction, ultrasonic-assistant extraction andhomogenization extraction, when added concentration was 0.1 mg·kg^-1, the range of recovery of thethree methods was 80%～120%, 70%～140%, 63%～130%, respectively,and the relative standarddeviation (RSD) were less than 9.2%. The minimum detection limits for the six sulfonamides was10μg·kg^-1 to 12μg·kg^-1. It was found that the ASE was a quickly and effectively extraction compared with the othertwo extraction, the extracting time was 23 min and the total analysis time needed 1.5h, the ASEwas fit for the detection of antibiotics residues in animal tissues.3. A high-performance liquid chromatography method for the detection of sulfonamidesresidues in eggs was established, and effect of sulfonamides residues in eggs during the heatingprocess was also determined.The egg samples were extracted with ethyl acetate by ultrasonic-assistant extraction, purifiedfrom fats with n-hexane, then analyzed in HPLC. The analysis conditions for sulfonamides in eggswere acquired. Hypersil ODS2 column; Mobile phase: methanol/0.08% acetic acid solution,V/V=38/62; Wavelength: 275nm; Flowing rate: 0.8mL·min^-1; Column temperature: roomtemperature; Injection volume: 10μL. When added concentration was 0.1mg·kg^-1, the recoveriesof six sulfonamides were 78.8%～103.0% and the RSD were less than 8.5%, the total analysis timewas 2 h, so the built method was fit for the detection of sulfonamide residues, and it was a accurate,rapid and sensitive measure. The result also indicated that sulfonamides in eggs obviouslydecreasing with the processing temperature and time increasing, this show that the thermal stabilityof sulfonamides was influenced by the processing temperature and time.