鸡肉冻干粉中妥曲珠利及妥曲珠利砜残留标准样品的研制

Preparation and Certification of Reference Materials for Toltrazuil and Toltrazuil Sulfone in Chicken Lyophilisates

建立了鸡肉冻干粉中妥曲珠利和妥曲珠利砜标准样品的研制和定值方法。通过口灌给药,使妥曲珠利在鸡体内代谢,从而使鸡肉中含有一定浓度的妥曲珠利和妥曲珠利砜,经均质、冷冻干燥、真空封装等处理后获得1批852个独立包装的鸡肉冻干粉标准样品。采用液相色谱-串联质谱对样品的均匀性和稳定性进行检测,通过8家实验室协作定值的方式对标准样品进行定值和不确定度评估,最终确定妥曲珠利的标准值为(60.42±9.12)μg/kg,妥曲珠利砜的标准值为(73.10±12.48)μg/kg。结果表明样品的均匀性良好,稳定性长达24个月,可用于鸡肉中妥曲珠利和妥曲珠利砜残留分析的质量控制。

A method for preparing and certifying the reference materials of tohrazuil and toltrazuil sul- lone in chicken muscle lyophilisates was presented. Tohrazuil was accessed to chicken by oral admin- istration. With the metabolism of toltrazuil in chiken, a certain concentration of toltrazuil and toltra- zuil sulfone were obtained in the muscles. Lyophilization of the muscles was performed in one batch, and 852 bags of samples were obtained by the procedure of homogenation, cryodesiccation and vacu- um - packaging. The homogeneity and stability of the sample were examined by high performance liq- uid chromatography - tandem mass spectrometry （ HPLC - MS/MS）. The value of the chemical con- stituent of the sample was certified through the collaborative analysis program participated by 8 labora- tories, and the uncertainty was evaluated. The standard values of standard samples were certified as （60.42± 9. 12 ）μg/kg for toltrazuil and （73.10 ±12.48 ）μg/kg for toltrazuil sulfone. The results showed that good homogeneity and stability of the sample reached up to 24 months, and could be used for the quality control of tohrazuil and toltrazuil sulfone residue in chicken.