Study On Analysis Method Of Veterinary Drug Residues In Animal-derived Food By Ultra Performance Liquid Chromatography-electrospray Ionization Tandem Mass Spectrometry

Recent years, food security events occurs frequently. It relates to not only the survival and health of individual, but also the diathesis, rise and fall of our nation, even more, it influences the state reputation in international trade directly. For the sake of Chinese physical fitness, and in order to provide strong technical support to our import and export trade, it has important practical sinificance to explore and perfect the residues analytical technique of harmful substance in food.The study used ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS), aimed at establishing a confirmative analytical method of sulfonamide and fluoroquinolone residues in animal origin foodstuff. The main contents included: Firstly, a confirmative method was developed by solid phase extraction combined with UPLC-ESI-MS/MS to detect 7 fluoroquinolone residues in chicken muscle simultaneously; Secondly, a confirmative method was developed by QuEChERS coupled with UPLC-ESI-MS/MS to detect 24 sulfonamide residues in bovine milk, Thirdly, a confirmative method was developed by QuEChERS coupled with UPLC-ESI-MS/MS to detect sulfonamide and fluoroquinolone residues in honey simultaneously.The results were as follows:1. The chicken muscle was extracted with acidified acetonitrile, defatted with n-hexane, and then purified by HLB solid phase extraction cartridge. The UPLC separation was performed on an ACQUITY UPLC^TM BEH C₁₈ column (50 mm×2.1 mm i.d. , 1.7μm) utilizing a gradient elution program of acetonitrile and water (containing 0.10% formic acid) as the mobile phase. Identification and quantification were achieved by using UPLC-ESI-MS/MS in positive mode and multiple reaction monitoring (MRM). Good linearities were observed in the range from 5μg/kg to 100μg/kg with correlation coefficients above 0.99. The method was validated at 5, 25 and 50μg/kg. The validation results were as follows: the average recoveries of 7 fluoroquinolones ranged from 79.2% to 108.6% with the relative standard deviations of 4.2%-8.9%. The detection limit of the method were 0.2-1.4μg/kg.2. The bovine milk sample were extracted and purified with the method of quick, easy, cheap, effective, rugged and safe (QuEChERS). The UPLC separation was performed on an ACQUITY UPLC^TMBEH C₁₈ column (100 mm×2.1 mm i.d. , 1.7μm) utilizing a gradient elution program of acetonitrile and water (containing 0.25% acetic acid) as the mobile phase. Identification and quantification were achieved by using UPLC-ESI-MS/MS in positive mode and multiple reaction monitoring (MRM). Good linearities were observed in the range from 5μg/kg to 100μg/kg with correlation coefficients above 0.99. The method was validated at 5, 25 and 50μg/kg. The validation results were as follows: the average recoveries of 24 antibiotics ranged from 60.5% to 110.9% with the relative standard deviations of 3.2%-13.1%. The detection limit of the method were 0.21-1.62μg/kg.3. The honey sample were extracted and purified with the method of quick, easy, cheap, effective, rugged and safe (QuEChERS). The UPLC separation was performed on an ACQUITY UPLC^TMBEH C₁₈ column (100 mm×2.1 mm i.d. , 1.7μm) utilizing a gradient elution program of acetonitrile and water (containing 0.15% formic acid) as the mobile phase. Identification and quantification were achieved by using UPLC-ESI-MS/MS in positive mode and multiple reaction monitoring (MRM). Good linearities were observed in the range from 5μg/kg to 100μg/kg with correlation coefficients above 0.99. The method was validated at 5, 25 and 100μg/kg. The validation results were as follows: the average recoveries of 16 antibiotics ranged from 80.3% to 107.3% with the relative standard deviations of 2.9%-8.9%. The detection limit of the method were 0.15-0.69μg/kg.With good reproducibility, high sensitivity, shorter analysis time and better determination capacity, the method could meet the requirements of both domestic and international legislation. The method is applicable to simultaneously confirm multi-residues of sulfonamide and fluoroquinolone residues in animal origin foodstuff.