摘要
目的:分析评定《食品安全国家标准水产品中土霉素、四环素、金霉素、多西环素残留量的测定》(GB 31656.11—2021)中第二法液相色谱-串联质谱法测定虾类中四环素、土霉素、多西环素和金霉素残留量的不确定度。方法:根据《测量不确定度的要求》(CNAS—CL01-G003:2021)和《化学分析中不确定度的评估指南》(CNAS—GL006:2019),采用GB 31656.11—2021中的液相色谱-串联质谱法测定虾类中四环素、土霉素、多西环素和金霉素的含量,通过建立不确定度的数学模型,对标准溶液的配制、标准曲线拟合、样品的前处理提取、样品的重复性实验等几个来源引入的不确定度进行计算分析。结果:在置信区间概率为P=95%时,金霉素测定结果为(18.6±2.0)μg·kg^(-1),k=2;多西环素测定结果为(18.8±1.9)μg·kg^(-1),k=2;土霉素测定结果为(19.3±1.9)μg·kg^(-1),k=2;四环素测定结果为(19.2±1.9)μg·kg^(-1),k=2。结论:测量结果的不确定度来源主要由标准曲线绘制引入,其次是由标准曲线拟合引入。因此,实验操作过程中通过优化标准曲线绘制和拟合可提高实验结果的准确度和可信度。
Objective:To analyze and evaluate the uncertainty of the determination of tetracycline,oxytetracycline,doxycycline and chlortetracycline residues in shrimp by the second method of liquid chromatography tandem mass spectrometry(LC-MS)in GB 31656.11—2021.Method:According to CNAS—CL01-G003:2011 and CNAS—GL006:2019,the contents of tetracycline,oxytetracycline,doxycycline and chlortetracycline in shrimp were determined by liquid chromatography tandem mass spectrometry(LC-MS)in GB 31656.11—2021.Through establishing the mathematical model of uncertainty,the uncertainty introduced from the preparation of standard solution,the fitting of standard curve,the pretreatment and extraction of samples,and the repeatability experiment of samples were calculated and analyzed.Result:When the confidence interval probability is P=95%,the determination result of chlortetracycline is(18.6±2.0)μg·kg^(-1),k=2;The determination result of doxycycline was(18.8±1.9)μg·kg^(-1),k=2;The determination result of oxytetracycline is(19.3±1.9)μg·kg^(-1),k=2;The determination result of tetracycline is(19.2±1.9)μg·kg^(-1),k=2.Conclusion:The uncertainty of measurement results is mainly derived from the drawing of standard curve,followed by the fitting of standard curve.Therefore,the accuracy and reliability of the experimental results can be improved by optimizing the standard curve drawing and fitting during the experimental operation.
作者
何咏欣
陈嘉欣
龚海锟
杨嘉鑫威
张辉
林泽珊
黄景初
钱振杰
HE Yongxin;CHEN Jiaxin;GONG Haikun;YANG Jiaxinwei;ZHANG Hui;LIN Zeshan;HUANG Jingchu;QIAN Zhenjie(Guangzhou Food Inspection Institute,Guangzhou 511400,China)
出处
《现代食品》
2022年第21期159-165,169,共8页
Modern Food
基金
广东省药品监督管理局科技创新团队项目(2019TDBB04)。
关键词
土霉素
四环素
金霉素
多西环素
液相色谱-串联质谱法
不确定度评定
oxytetracycline
tetracycline
chlortetracycline
doxycycline
liquid chromatography tandem mass spectrometry
uncertainty evaluation
