作者：尹太坤¹, 杨方², 刘正才², 林永辉²

作者单位：1. 福州大学石油化工学院, 福建 福州 350108;
2. 福建出入境检验检疫局检验检疫技术中心, 福建 福州 350001

关键词：基体标准物质;喹诺酮类药物;磺胺类药物;多残留;鳗鲡肌肉

摘要：

建立鳗鲡肌肉中8种喹诺酮类及磺胺类药物多残留基体标准物质的研制和定值方法。以一定浓度药浴给药,使药物在鱼体内自然代谢,从而使鳗鲡体内含有药物残留。经均质、真空包装及辐照处理后,获得一批420个独立包装的的鳗鲡肌肉样本。经均匀性和稳定性检验,由8家实验室采用液相色谱-串联质谱法对该样本进行协同定值,并进行不确定度评估。结果表明:样本中恩诺沙星、环丙沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹、磺胺二甲基嘧啶、磺胺间甲氧嘧啶的特性值分别为(34.342.69),(19.301.75),(39.143.08),(39.863.88),(15.001.05),(46.834.37),(27.172.74),(31.653.73)g/kg(k=2),均匀性及稳定性良好,适用于动物源食品中喹诺酮类、磺胺类药物检测过程的方法验证和检测结果质量控制。

Preparation of matrix reference material for quinolone and sulfonamide residues in eel muscle

YIN Taikun¹, YANG Fang², LIU Zhengcai², LIN Yonghui²

1. School of Chemical Engineering, Fuzhou University, Fuzhou 350108, China;
2. Technology Centre of Fujian Entry-exit Inspection and Quarantine Bureau, Fuzhou 350001, China

Abstract: A methodology for preparing and certifying the reference materials of 8 kinds of quinolone and sulfonamide drugs in eel muscle was introduced. The eels were dosed with a certain concentration of drugs. The metabolism of the drugs in vivo enabled the eel muscle to contain drug residues. A batch of 420 bags of eel muscle samples were obtained through homogenation, vacuum packing and irradiation. The homogeneity and stability of the samples were strictly examined. The concentrations of each chemical constituent in the samples were collaboratively analyzed by 8 laboratories using liquid chromatography-tandem mass spectrometry and their uncertainty was assessed. The results show that the characteristic values of the enrofloxacin,ciprofloxacin hydrochloride,ofloxacin, norfloxacin,oxolinic,flumequine, sulfamethazine, sulfamonomethoxine characteristics in these samples are (34.34±2.69), (19.30±1.75), (39.14±3.08), (39.86±3.88), (15.00±1.05), (46.83±4.37), (27.17±2.74), (31.65±3.73)μg/kg(k=2) respectively, high in uniformity and stability. The methodology is suitable for verifying the methods in the inspection process of quinolone and sulfonamide drugs in animal-derived foodstuffs and for controlling the quality of the inspection results.

Keywords: the matrix reference material;quinolones;sulfonamides;multi residues;eel muscle

2016, 42(4): 54-59  收稿日期: 2015-09-20;收到修改稿日期: 2015-11-13

基金项目: 质检公益项目(201310143-02);福建省科技重点项目(2012Y6001);福建检验检疫局科技计划项目(FK2010-23)

作者简介: 尹太坤(1988-),男,山东德州市人,硕士研究生,专业方向为食品安全分析。

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