摘要
为填补我国尼卡巴嗪药物残留基体标准样品的空白,建立了鸡肉中尼卡巴嗪残留基体标准样品的研制方法。通过在饲料中添加尼卡巴嗪药粉喂养白羽肉鸡,使药物在鸡体内自然代谢,得到尼卡巴嗪残留阳性动物。取鸡前胸肉制成肉糜,经均质、冷冻干燥、粉碎、筛分、包装、辐照灭菌等处理,制备了355份含有尼卡巴嗪残留的鸡肉冻干粉。按照国家标准样品的规范,进行了均匀性检验、稳定性检验、定值和不确定度分析。采用液相色谱-串联质谱法(LC-MS/MS)测定样品中的尼卡巴嗪含量,以8家具有资质的实验室进行协同定值。结果表明本批标准样品的均匀性和稳定性良好,在-70、4、25、50℃下能稳定保存14天,在-18℃下保存的稳定性可达12个月,符合国家标准样品的相关要求。最终确定标准样品中尼卡巴嗪的标准值为(157.7±11.0)μg·kg^(-1)(k=2)。该标准样品可用于尼卡巴嗪的检测方法优化、检测实验室的能力评价,对于食品中尼卡巴嗪残留检测具有重要意义。
A development method for nicarbazin residue matrix reference materials in chicken muscle was established in this paper to fill the gap of those in China.Positive animals with nicarbazin residues were obtained by feeding white feather broiler chickens with nicarbazin drug powder in feed and allowing the drug to metabolize naturally in the chickens.A batch of 355 chicken lyophilized powders containing nicarbazin residues were prepared by taking chicken breast meat and making minced meat,through the processes of homogenization,freeze-drying,crushing,sieving,packaging and irradiation sterilization.Homogeneity assessments,stability monitoring,characterization and uncertainty analysis were carried out according to the requirements of national reference materials.The contents of nicarbazin in the samples were determined by liquid chromatography-tandem mass spectrometry(LC-MS),which were cooperatively certified by 8 expert laboratories.The results showed that the homogeneity and stability of this batch of reference materials were good and they could be kept stable for 14 days under the temperature conditions of -70℃,4℃,25℃and 50℃,and up to 12 months when stored at -18℃,which was in accordance with the relevant requirements of the national reference materials.The certified value of nicarbazin in the reference materials was finally determined to be (157.7±11.0)μg·kg^(-1)(k=2).The reference material could be used for optimization of detection methods for nicarbazin,and capacity evaluation on nicarbazin residue testing laboratories,which is of great significance to the detection of nicarbazin residues in food.
作者
林永健
徐敦明
沈鹭英
刘正才
李雨哲
王伟
肖晶
LIN Yong-jian;XU Dun-ming;SHEN Lu-ying;LIU Zheng-cai;LI Yu-zhe;WANG Wei;XIAO Jing(College of Food Science,Fujian Agriculture and Forestry University,Fuzhou 350002,China;Technical Center of Xiamen Customs,Xiamen 361026,China;Technical Center of Fuzhou Customs,Fuzhou 350001,China;China National Center for Food Safety Risk Assessment,Beijing 100022,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第2期166-172,共7页
Journal of Instrumental Analysis
基金
国家重点研发计划项目(2020YFF0305002)
福州海关科研项目(FK2021-17)
分析标准样品的研制计划项目(S2019322)。
