超高效液相色谱质谱法同时测定水产品中58种药物残留  

Simultaneous determination of 58 drug residues in aquatic products by UPLC-MS/MS

作　　者：吴丹 林英扬 张杨 肖曼 魏芝芝 张微 徐媛原 李凯华 张兵 WU Dan;LIN Yingyang;ZHANG Yang;XIAO Man;WEI Zhizhi;ZHANG Wei;XU Yuanyuan;LI Kaihua;ZHANG Bing(Shenzhen Inspection and Testing center of Quality and Safety of Agricultural Products,Shenzhen 518101)

机构地区：[1]深圳市质量安全检验检测研究院,广东深圳518055

出　　处：《中国渔业质量与标准》2024年第6期1-9,共9页Chinese Fishery Quality and Standards

摘　　要：本研究基于超高效液相色谱质谱法(UPLC-MS/MS)建立了一种可同时快速测定水产品中喹诺酮类、苯二氮卓类、β-受体激动剂类、苯并咪唑类、硝基咪唑类、糖皮质激素类、非甾体抗炎药类、磺酰脲类8类药物58种药物残留的检测方法。方法前处理使用80%乙腈水溶液(含0.2%甲酸)一次提取,Waters PRiME HLB固相萃取小柱净化除杂,经高效液相色谱—串联质谱(HPLC-MS/MS)测定,基质匹配标准工作曲线定量。该定量方法中58种兽药的基质标准曲线线性良好,R^(2)均大于0.99;3种浓度加标水平下,相对标准偏差为1.9%~14.7%,平均回收率为78.9%~112.8%。应用该方法对市售30份水产品进行检测,在9份样品中检出喹诺酮类药物,检出量为2.23~425.00μg/kg。本方法简单、快速,可适用于水产品中多类药物残留的同时检测筛查,并为后续水产品安全监测高通量方法的开发提供参考。[中国渔业质量与标准,2024,14(6):01-09]An ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method was established for the simultaneous detection of 58 drug residues across 8 categories in aquatic products,including quinolones,benzodiazepines,β-receptor agonist,nitroimidazoles,benzimidazoles,glucocorticoids,nonsteroidal anti-inflammatory drugs,and sulfonylureas.The samples were extracted by 80%acetonitrile aqueous solution(containing 0.2%formic acid)and purified using a Waters PRiME HLB solid-phase extraction column.The analytes were quantified by high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)with a matrix-matched standard curve.The correlation coefficients for all 58 veterinary drugs were greater than 0.99.At three spiked concentration levels,the relative standard deviations ranged from 1.9%to 14.7%,and the average recovery rates were between 78.9%and 112.8%.The method was applied to 30 commercially available aquatic samples,where quinolones were detected in 9 samples at levels ranging from 2.23 to 425.00μg/kg.The method is simple,fast,and suitable for the simultaneous detection and screening of multiple drug residues in aquatic products.It also serves as a reference for the development of high-throughput methods for the safety monitoring of aquatic products.[Chinese Fishery Quality and Standards,2024,14(6):01-09]

关 键 词：高效液相色谱—串联质谱法 水产品 药物残留 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]