摘要
基于QuEChERS结合高效液相色谱-串联质谱法建立了渔用中草药散剂中测定喹诺酮类和磺胺类药物残留的检测方法。从提取溶剂、提取溶剂用量、净化剂以及净化剂用量4方面对QuEChERS方法进行优化,采用内标法定量,最终选择回收效果最佳的方法条件。结果显示,氧氟沙星、恩诺沙星、丹诺沙星、洛美沙星、双氟沙星、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺间甲氧嘧啶、磺胺邻二甲氧嘧啶、磺胺间二甲氧嘧啶、磺胺甲噻二唑、磺胺氯哒嗪、磺胺甲恶唑、磺胺喹恶啉这14种抗生素在2~200 ng/mL线性良好,相关系数R^(2)均大于0.99,定量限均为1.0μg/kg,3个浓度添加水平(1、25和50μg/kg)下14种抗生素的平均回收率为72.5%~123.5%,相对标准偏差为0.9%~12.9%。本方法具有前处理简单、快速、准确、灵敏度高和选择性强等优点,适用于渔用中草药散剂中喹诺酮类和磺胺类药物残留的快速检测。
A method for determining quinolone and sulfonamide antibiotic residues in Chinese herbal powder for fishery has been established using the QuEChERS technique combined with high-performance liquid chromatography-mass spectrometry(HPLC-MS/MS).The QuEChERS method was optimized across four key aspects:extraction solvent,extraction solvent volume,purification agent,purification agent volume,and other relevant factors.Quantify using the internal standard method,and ultimately select the method conditions that yield the best recovery results.The results showed that the 14 antibiotics tested—namely,ofloxacin,enrofloxacin,lomefloxacin,difloxacin,sulfamethoxypyrimidine,sulfamethoxypyrimidine,sulfadimethoxypyrimidine,sulfamethoxypyrimidine,sulfamethoxazole,sulfamethoxazole,and sulfaquinoxaline—exhibited excellent linearity within the concentration range of 2 to 200 ng/mL,with the correlation coefficients(R^(2))exceeding 0.99,and the quantitative limits all set at 1.0μg/kg.The average recoveries of these 14 antibiotics at three concentration levels(1μg/kg,25μg/kg,and 50μg/kg)ranged from 72.5%to 123.5%,with the relative standard deviations of 0.9%to 12.9%.The method is characterized by its simplicity,rapidity,accuracy,high sensitivity,and selectivity,making it highly suitable for rapidly detecting of quinolone and sulfonamide residues in Chinese herbal powder used in the fishery industry.
作者
位绍红
钱卓真
汤水粉
王丽娟
WEI Shaohong;QIAN Zhuozhen;TANG Shuifen;WANG Lijuan(Fisheries Research Institute of Fujian,Key Laboratory of Cultivation and High-value Utilization of Marine Organisms in Fujian province,Xiamen 361013,China)
出处
《中国渔业质量与标准》
2024年第4期28-35,共8页
Chinese Fishery Quality and Standards
基金
福建省省属公益类科研院所基本科研专项(2021R10130012)。
