基于低共熔溶剂高效萃取液质联用快速定量检测养殖水中氯霉素类抗生素残留方法的研究  

Research on Rapid Quantitative Determination of Chloramphenicol Antibiotics and Veterinary Drug Residues in Aquaculture Water Based on Deep Eutectic Solvents High Performance Extraction Liquid Chromatography-Mass Spectrometry

作　　者：李凯华 张杨 徐媛原 张微 肖曼 林敏霞 林英扬 吴丹 魏芝芝 张兵 LI kaihua;ZHANG Yang;XU Yuanyuan;ZHANG Wei;XIAO Man;LIN minxia;LIN Yingyang;WU Dan;WEI Zhizhi;ZHANG Bing(Shenzhen Institute of Quality and Safety Inspection and Research,Shenzhen 518055,Guangdong China)

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：《饲料博览》2023年第3期25-30,共6页Feed Review

摘　　要：为建立一种养殖水中氯霉素类抗生素残留的微量低共熔溶剂高效萃取液质联用快速定量检测的方法,将养殖水经滤纸过滤,取10 mL水样,加入适量内标物质,混匀取1 mL水样置于微量离心管中,加入适量低共熔溶剂,旋涡混匀静置提取上层清液,用乙腈定容至1 mL,过0.22μm滤膜,然后用高效液相色谱进行分离,电喷雾串联四级杆质谱进行检测,用内标物进行定量。结果显示:氯霉素的线性范围为0.1~5.0μg·kg^(-1),相关系数为0.999 4,平均检出限达到0.005 3μg·kg^(-1),方法的回收率为80.3%~103.6%,相对标准偏差为3.5%~8.3%;氟苯尼考的线性范围为1.0~20.0μg·kg^(-1),相关系数为0.999 8,平均检出限达到0.022 8μg·kg^(-1),方法的回收率为63.4%~85.2%,相对标准偏差为2.2%~6.2%。结果表明该方法萃取及检测试剂消耗少、时间短、灵敏度高、准确性好,适用于养殖水中氯霉素类抗生素的检测。To establish a rapid and quantitative method for the determination of chloramphenicol antibiotics residues in aquaculture water by liquid chromatography mass spectrometry(LC-MS)with micro eutectic solvent extraction and enrichment,the culture water was filtered by filter paper,10 mL of water sample was added with proper amount of internal standard substance,1 mL of water sample was mixed evenly in a micro-centrifuge tube,adding proper amount of eutectic solvent,vortex mixing and standing to extract the top layer clear liquid,acetonitrile was fixed to 1 mL,and filtered by 0.22μm.The sample was separated by high-performance liquid chromatography,and the internal standard was quantified by electrospray ionization tandem mass spectrometry.The results showed the linear range of chloramphenicol was 0.1-5.0μg·kg^(-1),and the correlation coefficient was 0.9994.The average detection limit of chloramphenicol was up to 0.0053μg·kg^(-1).The recovery of chloramphenicol was 80.3%-103.6%,the relative standard deviation was between 3.5%and 8.3%.The linear range of the florfenicol was 1.0-20.0μg·kg^(-1),and the correlation coefficient was 0.9998.The average detection limit of the florfenicol was up to 0.0228μg·kg^(-1).The recoveries of the method ranged from 63.4%to 85.2%,the relative standard deviation was between 2.2%and 6.2%.The results showed that method had the advantages of less consumption of extraction and detection reagent,short time,high sensitivity and good accuracy.This method was proved to be suitable for the detection of chloramphenicol in aquaculture water,and provided a clear research direction for the next step of using low eutectic solvent extraction in aquaculture environment and detection of veterinary drug residues in aquatic products.

关 键 词：低共熔溶剂 萃取 养殖水 氯霉素类抗生素 液质联用 

分 类 号：S859.796[农业科学—临床兽医学]