三穗鸭中磺胺类和喹诺酮类药物残留检测及风险评估

建立了15种磺胺类和6种氟喹诺酮类药物残留的超高效液相色谱法-串联质谱法,并采用此法对2018年贵州省三穗县三穗鸭肉进行了15种磺胺类和6中氟喹诺酮类药物残留检测,在此基础上对三穗鸭肉产品中的磺胺类和氟喹诺酮类药物的残留风险进行了分析。结果显示,21种药物在5~200 μg/L质量浓度范围内线性关系良好,决定系数(R²)均大于0.990,药物的检出限为0.5~2.0 μg/kg,定量限2.0~5.0 μg/kg,在添加浓度5~50 μg/kg的范围内,21种药物回收率为70.3%~113.2%,相对标准偏差为2.1%~11.5%(n=6),该方法简单、快捷、精密度和准确度高,能满足鸭肉中两类兽药检测;三穗鸭肉中氟喹诺酮类均未检出,磺胺类仅检出磺胺氯哒嗪,检出率2.17%,检出值为2.37~3.68 μg/kg,均值3.33 μg/kg,未超过国家规定限量(100 μg/kg),其余磺胺类指标均未检出;参照国际上磺胺类ADI值规定,三穗鸭肉中磺胺氯哒嗪的食品安全指数值平均值为0.00014,最小值为0.00010,最大值为0.00016,均远远低于1;结果均表明,三穗鸭肉中氟喹诺酮类和磺胺类药物残留对人体的潜在危害水平是可以接受的。

Residues Detection and Risk Assessment of Sulfonamides and Fluoroquinolones Drugs in the Sansui Duck

Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for the detection of 15 kinds of sulfonamides and 6 kinds of fluoroquinolones residues in the Sansui duck. Based on this method,the residual risks of 21 analytes were evaluated. The standard curve for 21 analytes showed a good linear relationship with the concentration range of 5~200 μg/L,correlation coefficient were more than 0.990,and the limit of detection(LOD)were 0.5~2.0 μg/kg,limit of quantitation(LOQ)were 2.0~5.0 μg/kg,and the recovery rate were 70.3%~113.2%,and relative standard deviation(RSD)were 2.1%~11.5%(n=6)when the amount was 5~50 μg/kg. This method was simple,quick,with a better precision,higher accuracy,and could be applied to detect the two types of veterinary drug residues in duck. No fluoroquinolones drugs in the Sansui duck were detected. The results showed that the sulfachloropyridazine residues belonged to sulfonamides were at a rate of 2.17%,ranged from 2.37 μg/kg to 3.68 μg/kg with an average value of 3.33 μg/kg,not exceeding the maximum residue limits set by the state(100 μg/kg),and other sulfonamides were not detected. Refer to the international regulations on ADI value of sulfonamides,the average value of food safety index in sansui duck products related to sulfachloropyridazine residues was 0.00014,the minimum value was 0.00010,the maximum was 0.00016,which was far below 1.It showed that the potential hazard level of the fluoroquinolones and sulfonamides residues in sansui duck is acceptable.