草鱼肌肉中呋喃唑酮代谢物AOZ检测能力验证样品的制备研究

Preparation and study on the proficiency testing samples of furazolidone metabolite AOZ residual in Grass carp

为解决现行水产品药物残留检测能力验证样品制备方式单一,现用能力验证样品实际检测分析难度与真实样品之间存在差距的现实问题,实验采用药浴给药的方式,研究了水温、药浴时间等因素对草鱼肌肉中AOZ残留浓度的影响。结果显示:在水温25℃、鱼体规格900~1 100 g、药浴10 h的条件下,草鱼肌肉中AOZ含量变化相对平稳,确立的药浴初始浓度x(μg/L)与草鱼肌肉中残留的AOZ浓度y(μg/kg)之间简单关式为y=0.22x。在此条件下制备了AOZ残留浓度为10.0μg/kg的能力验证样品,采用液相色谱-串联质谱法对样品的均匀性和稳定性进行了评价。样品检测结果均匀性和稳定性良好,符合能力验证样品的要求。

The effects of water temperature,bath time and other factors on the residual concentration of furazolidone metabolites in Grass carp muscle were studied by means of drug bath administration to solve the problem of the sample preparation method is simple of proficiency testing.Meanwhile,the practical detection and analysis difficulty problem of the gap between the current proficiency testing samples and the real samples were also research objectives..The results showed that the change of AOZ content in the muscle of the grass carp was relatively stable under the conditions of water temperature 25℃,fish size ranged from 900 to 1100g and drug bath time 10 h.The relationship between initial concentration of drug bath x(μg/L)and the residual AOZ in muscle concentration y(μg/kg)is y=0.22 x,The homogeneity and stability of the prepared sample were detected by liquid chromatography-tandem mass spectrometry.The sample has a good homogeneity,stability and meets the requirements of proficiency testing.