超高效液相色谱-串联质谱法检测卤肉中36种兽药残留  

Determination of 36 Veterinary Drug Residues in Cooked Meat by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：张飞 王远[1] 马小宁[1] 张金磊 巩婧婷 付明鑫[1] ZHANG Fei;WANG Yuan;MA Xiaoning;ZHANG Jinlei;GONG Jingting;FU Mingxin(Analysis and Testing Center,Xinjiang Academy of Agricultural Reclamation Science,Shihezi 832000,China)

机构地区：[1]新疆农垦科学院分析测试中心,新疆石河子832000

出　　处：《食品工业科技》2023年第13期340-348,共9页Science and Technology of Food Industry

摘　　要：建立了卤肉中金刚烷胺、磺胺类、喹诺酮类及氯霉素类等36种兽药残留的检测方法。卤肉样品通过乙腈-水溶液(V:V=8:2)提取,PRiME HLB固相萃取柱净化,配有电喷雾离子源(ESI±)的超高效液相色谱-串联质谱(UPLC-MS/MS),在正负离子多反应监测(MRM)模式下同时测定,基质匹配标准曲线定量。结果表明,所研究的36种兽药在0.5~20.0 ng/mL浓度范围内均呈良好线性关系(R2>0.999)。本方法中36种药物的检出限均为0.10μg/kg,定量限均为0.33μg/kg,在高中低3个不同浓度(0.5,1.0和5.0μg/kg)36种兽药的添加回收率为70.8%~106.9%,相对标准偏差(RSD,n=6)0.2%~6.2%。该研究建立的方法操作简单、准确性高、回收率和重现性好,可同时对卤肉中的36种兽药残留进行测定。A method was developed for the determination of amantadine sulfonamides,quinolones and chloramphenicols in cooked meat.The samples were extracted with acetonitrile-water mixtures(V:V=8:2),purified with PRiME HLB solid phase extraction column.36 veterinary drugs were determined by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with an electrospray ion source(ESI±)in positive and negative ion switching scanning mode.The results showed that the 36 veterinary drugs showed a good linear relationship in the concentration range of 0.5~20.0 ng/mL(R2>0.999).The limits of detection were 0.10μg/kg and the limits of quantitation were 0.33μg/kg.The average recovery was 70.8%~106.9%in the range of high,medium and low concentrations(0.5,1.0 and 5.0μg/kg).The relative standard deviations(RSD,n=6)was 0.2%~6.2%.The method is simple,sensitive and accurate,and could be used for the determination of 36 veterinary drug residues in cooked meat.

关 键 词：超高效液相色谱-串联质谱法 卤肉 PRIME HLB 固相萃取 兽药残留 

分 类 号：O657.63[理学—分析化学]