1.福建农林大学 食品科学学院,福建 福州 350002
2.厦门海关技术中心,福建 厦门 361026
3.福州海关技术中心,福建 福州 350001
4.国家食品安全风险评估中心,北京 100022
刘正才,硕士,研究员,研究方向:农兽药残留检测分析,E-mail:54369174@qq.com
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林永健,徐敦明,沈鹭英等.鸡肉中尼卡巴嗪残留基体标准样品的研制[J].分析测试学报,2023,42(02):166-172.
LIN Yong-jian,XU Dun-ming,SHEN Lu-ying,et al.Preparation of Matrix Reference Material for Nicarbazin Residues in Chicken Muscle[J].Journal of Instrumental Analysis,2023,42(02):166-172.
林永健,徐敦明,沈鹭英等.鸡肉中尼卡巴嗪残留基体标准样品的研制[J].分析测试学报,2023,42(02):166-172. DOI: 10.19969/j.fxcsxb.22090101.
LIN Yong-jian,XU Dun-ming,SHEN Lu-ying,et al.Preparation of Matrix Reference Material for Nicarbazin Residues in Chicken Muscle[J].Journal of Instrumental Analysis,2023,42(02):166-172. DOI: 10.19969/j.fxcsxb.22090101.
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.
鸡肉尼卡巴嗪基体标准样品液相色谱-串联质谱法(LC-MS/MS)
chickennicarbazinmatrix reference materialliquid chromatography-tandem mass spectrometry(LC-MS/MS)
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