摘要
评定不同高效液相色谱-串联质谱仪(HPLC-MS)测定猪肉中环丙沙星、恩诺沙星残留量的不确定度。依据GB/T 21312-2007,分别采用Thermo TSQ Quantiva型及Agilent G6470B型高效液相色谱-串联质谱仪测定猪肉中环丙沙星和恩诺沙星残留量,构建评估模型并分析检测过程。结果:当Thermo TSQ Quantiva型测定环丙沙星、恩诺沙星残留量分别为62.91、423.87μg/kg时,其扩展不确定度分别为30.20、36.45μg/kg, k=2;当Agilent G6470B型测定环丙沙星、恩诺沙星残留量分别为61.29、424.87μg/kg时,其扩展不确定度分别为38.00、46.74μg/kg, k=2。结果表明,检测过程的不确定度主要来源于标准工作曲线拟合。且ThermoTSQ Quantiva型测定引入的相对不确定度小于Agilent G6470B测定引入的相对不确定度,更为稳定。
To evaluate the uncertainty of determination of ciprofloxacin and enrofloxacin residues in pork by different high performance liquid chromatography-tandem mass spectrometry(HPLC-MS). According to GB/T 21312-2007, we used Thermo TSQ Quantiva and Agilent G6470 B high-performance liquid chromatography-tandem mass spectrometers to determine the residues of ciprofloxacin and enrofloxacin in pork, construct an evaluation model and analyze the detection process. The residual amounts of ciprofloxacin and enrofloxacin measured by Thermo TSQ Quantiva were 62.91 and 423.87 μg/kg, and their expanded uncertainties were 30.20 and 36.45 μg/kg, k=2, respectively;Agilent G6470 B type determined ciprofloxacin, enrofloxacin residues were 61.29, 424.87 μg/kg, and their expanded uncertainties were 38.00, 46.74 μg/kg, k=2, respectively. The results show that the uncertainty of the detection process mainly comes from the standard working curve fitting. Moreover, the relative uncertainty introduced by the ThermoTSQ Quantiva-type assay is less than that introduced by the Agilent G6470 B assay, which is more stable.
作者
李小红
张亚锋
张潇
梁红月
李荣
徐瑞婕
刘皖臻
LI Xiao-hong;ZHANG Ya-feng;ZHANG Xiao;LIANG Hong-yue;LI Rong;XU Rui-jie;LIU Wan-zhen(Xi'an Institute for Food and Drug Control,Xi'an,Shaanxi 710054,China)
出处
《畜牧兽医杂志》
2022年第6期4-9,18,共7页
Journal of Animal Science and Veterinary Medicine
基金
陕西省科技资源开放共享平台项目(2021PT-044)。
关键词
高效液相色谱/串联质谱法
环丙沙星
恩诺沙星
不确定度
high performance liquid chromatography/tandem mass spectrometry
ciprofloxacin
enrofloxacin
uncertainty