鸡肉冻干粉中磺胺类药物残留标准物质的研制

Preparation of Chicken Lyophilized Powder Matrix Reference Material Containing Sulfonamides

建立一种制备以鸡肉为基质的磺胺类药物标准物质的制作方法。鸡肉样品经斩拌、加标、冷冻干燥、粉碎、混匀、真空包装后,参考GB/T 21316—2007《动物源性食品中磺胺类药物残留量的测定液相色谱-质谱/质谱法》考察冻干法对样品的均匀性、稳定性影响,并联合多家实验室对鸡肉中磺胺类药物基质样品定值,同时分析样品的不确定度。结果表明,F-检验法和t-检验法表明在95%置信区间内,冻干法制备的样品均匀性、短期稳定性和长期稳定性均达到标准物质要求。采用格拉布斯和柯克伦检验对定值结果进行异常值检验,并对结果进行不确定度评估,冻干粉样品磺胺甲基嘧啶定值结果为209.7μg/kg,不确定度为5.9μg/kg;冻干粉样品磺胺二甲基嘧啶定值结果为447.1μg/kg,不确定度为13.2μg/kg。冻干法制备的样品具有良好的均匀性、稳定性,可作为肉类冻干粉中磺胺类药物含量检测使用的标准物质。

Establish a preparation method for sulfonamides reference materials using chicken lyophilized powder as a substrate.After the chicken samples were cut,labeled,freeze-dried,ground,mixed and vacuum-packed,the uniformity and stability of the samples were tested by GB/T 21316—2007,the values of sulfonamides matrix samples with cucumber freezedried powder were determined together with several laboratories,and the uncertainty of the samples was analyzed.The results showed that the F-test and t-test methods showed that within the 95% confidence interval,sample uniformity,short-term stability and long-term stability met the requirements of standard materials.The outliers of the fixed value results were tested by Grubbs and Cochrane tests,and the uncertainty of the results was evaluated.The fixed value of the sulfamethazine form sample was 209.69μg/kg and the uncertainty was 5.86μg/kg;The fixed value of the sulfamethazine form sample was 447.06μg/kg and the uncertainty was 13.24μg/kg.The sample had good uniformity and stability,and could be used as a standard substance for the detection of sulfonamides content in meat lyophilized powder.