| β-lactam antibiotic refers to the antibiotic which containsβ-lactam ring. It has become the most applied kind of antibiotic in the medical prevention and treatment for animal diseases up until now. However, with improper usage such as not following the withdrawal time, this kind of antibiotic can be left in animal-derived food. Therefore, it is a must-do task to reinforce effective test and monitor for the antibiotic residual in the animal-derived food so as to safeguard people's food safety.The purpose of this paper is to research the method of multi-residue detection theβ-lactam antibiotics in the food of animal origin. Through optimization the pretreatment method of food of animal origin, and establishment the method of detection the residues ofβ-lactam antibiotics in the food of animal origin by high performance liquid chromatography.Paper was divided into the five parts:Chapter 1:Introduction of the type of antibiotics and the structural of theβ-lactam antibiotics, reviewed the development of the analysis methods of antibiotic residues, as well as, the principles of the preparation methods of the animal origin food samples,characteristics,application. It was also summarized the status of veterinary drug residues in China and the analysis progress of theβ-lactam antibiotic residues in food of animal origin.The paper identified its topic selection on this basis of this review.Chapter 2:As the study objectives of the nineβ-lactam, the pretreatment conditions were optimized:In this study, protein precipitation with acetonitrile, phosphate buffer as extraction solution, the use of ultrasonic assisted extraction by 20kHz in 5 min,centrifuged,purificated by solid phase extraction column,using Agilent TC C18 column (150 mm×4.6 mm id,5μm), the choice of phosphate-methanol as mobile phase gradient elution, flow rate 1.0 mL/min,220 nm detection, separation and detection within 22 minutes, the nine of antibiotics have good linearity in 1～100μg/mL, the limits of detection between 0.5-2.5μg/L. By ultrasound assisted extraction, the detection limit was improved effectively, and the realization of multi-residue detection theβ-lactam antibiotics in the food of animal origin by the conventional liquid. Chapter 3:A high performance liquid chromatographic(HPLC) method was developed for the determination of two penicillins residues in milk based on the formation of a stable complex between copper ions and penicillins under a certain conditions. The sample was extracted and degreased by acidified acetonitrile. The separation of two kinds of penicillin antibiotics was performed in 5 minutes on a Agilent TC C18 (150 mm×4.6 mm i.d.,5μm), with methanol-water as mobile phase at flow rate of 1.5 mL/min. The detection wavelength was set at 320 nm. The calibration curves were linear over the concentration range of 0.05-1.0 mg/L for penicillin G and 0.08-2.1 mg/L for ampicillin, with correlation coefficients of 0.9956 and 0.9984, respectively. The detection limits of penicillin G and ampicillin were 1.5×10-5 g/L and 2.4×10-5g/L, respectively, and relative standard deviations(RSD, n=5) were 2.4% and 1.8%. The effect of metal ions on separation of penicillins were also studied. The method showed high selectivity and sensitivity, and was suitable for the detection of penicillin in milk sample.Chapter 4:A new method, which was to link ammonium sulfate/polyethylene glycol aqueous two phase extraction system and high-performance liquid, to test several kinds of cephalosporin in the honey was created. In this study, optimization of aqueous two-phase extraction technique, combined with high performance liquid chromatography, the use of potassium dihydrogen phosphate-acetonitrile gradient elution separated in 7 minutes within three cephalosporins. A new method was established, simple steps, high sensitivity to detect cephalosporin residues in honey.Chapter 5:The entire paper was summarized. |
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