高效液相色谱法测定鸡蛋中25种咪唑类兽药及其代谢物残留OA北大核心CSTPCD
Determination of 25 Imidazole Veterinary Drugs and Their Metabo-lites in Eggs by High Performance Liquid Chromatography
建立了高效液相色谱(HPLC)测定鸡蛋中25种咪唑类兽药及其代谢物残留的分析方法.鸡蛋液经乙腈提取并浓缩后,采用Oasis PRIME HLB固相萃取柱净化,以甲醇和水为流动相进行梯度洗脱,采用ZORB-AXSB-Aq(250mm×4.6mm,5 μm)色谱柱分离,二极管阵列检测器(DAD)检测,外标法定量.实验结果表明,25种目标化合物在各自质量浓度范围内线性关系良好,相关系数(r2)均大于0.999,检出限(LOD)和定量下限(LOQ)分别为0.8~5.0 μg/kg和2.5~12.5 μg/kg.在低、中、高3个浓度水平下进行加标回收实验,平均加标回收率为78.5%~103%,相对标准偏差(RSD)为1.1%~6.5%.该方法无明显基质效应、准确度高、精密度好,可用于鸡蛋中25种咪唑类兽药及其代谢物的日常检测.
The method for the determination of 25 imidazole veterinary drugs and their metabolites in eggs was established by high performance liquid chromatography(HPLC).The egg solution was ex-tracted and concentrated by acetonitrile,purified by Oasis PRIME HLB solid phase extraction col-umn.The samples were eluted by gradient with methanol and water as mobile phases,separated by ZORBAX SB-Aq(250 mm×4.6 mm,5 μm)column,detected by diode array detector(DAD),and quantified by external standard method.The results demonstrated that the 25 compounds showed good linear relationships in their linear ranges with the correlation coefficients(r2)greater than 0.999.And the limits of detection(LODs)and quantification(LOQs)were 0.8-5.0 p.g/kg and 2.5-12.5 μg/kg,respectively.The average recoveries ranged from 78.5%to 103%and the relative stan-dard deviations(RSDs)ranged from 1.1%to 6.5%at three concentration levels.The method has no obvious matrix effect with high accuracy and good precision,which can be used for the daily detec-tion of 25 imidazole veterinary drugs and metabolites residues in eggs.
邱月;余秋玲;谭超兰;陆嘉莉;杨倩
重庆市计量质量检测研究院,重庆 401123
化学
苯并咪唑硝基咪唑代谢物高效液相色谱法鸡蛋
benzimidazolenitroimidazolemetabolitehigh performance liquid chromatographyegg
《分析测试学报》 2024 (007)
1018-1024 / 7
重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001);国家市场监督管理总局科技计划项目(2023MK106);重庆市市场监督管理局科研计划项目(CQSJKJ2022040,CQSJKJDW2023003)
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