摘要 建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时检测鸡蛋、液态奶、鸡肉及淡水鱼中4类(氯霉素类、硝基咪唑类、林可酰胺类与大环内酯类)8种禁限兽药与3种代谢物残留的分析方法。对样品前处理及色谱条件进行优化,样品经0.1 mol/L pH 9.0的磷酸盐缓冲液水解分散,乙腈提取,提取液经乙酸乙酯萃取后浓缩至近干,残留物用0.3 mL甲醇溶解,再加入5.7 mL磷酸盐缓冲液,混匀,溶解液经Oasis HLB固相萃取柱净化后上机分析,以甲醇与0.1%甲酸水溶液作为流动相进行梯度洗脱,经ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,采用ESI+和ESI-电离,在多反应监测模式下采集,同位素内标法定量。结果表明,11种待测物在色谱柱上完全基线分离,在各自范围内线性关系良好,相关系数(R2)>0.99,方法的检出限(LOD)为0.050~0.50μg/kg,定量限(LOQ)为0.20~1.5μg/kg。各待测物的平均回收率为65.3%~108%,相对标准偏差(RSD)为0.40%~21%。将该方法应用于市售样品中上述4类兽药残留的常规监测,其阳性样本的检测结果与标准方法测定结果无显著性差异。该方法灵敏度高,稳定性好,定量准确,适用于动物源性食品中多种禁限兽药及代谢物残留的同时快速测定。 Chloramphenicols,nitroimidazoles,lincosamides,and macrolides are common antibiotics used in veterinary medicine.Overdoses of these drugs will lead to residual substances in animal-derived foods and accumulate in the body through the food chain,thereby exerting adverse effects on human health.Therefore,regulation of veterinary drug levels is imperative to ensure the quality of animal-derived foods and safeguard the health of consumers.In this study,a method based on ultra performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction(SPE-UPLC-MS/MS)was developed for the simultaneous determination of eight prohibited and restricted veterinary drugs and three metabolite residues across four categories(chloramphenicols,nitroimidazoles,lincosamides,and macrolides)in eggs,liquid milk,chicken,and freshwater fish.The main factors affecting the response,recovery,and sensitivity of the method,such as the type and pH values of the extraction solvent,dilution solution for the analytes,type of chromatographic column,and type and proportion of the mobile phase,were optimized during sample pretreatment and instrument analysis.The samples were hydrolyzed and dispersed in 0.1 mol/L phosphate buffer solutions(pH 9.0)and extracted with acetonitrile.The extract was further extracted using ethyl acetate.After centrifugation,the supernatant ethyl acetate was concentrated to near dryness in nitrogen below 40℃.The residue was dissolved in 0.3 mL methanol,followed by the addition of 5.7 mL phosphate buffer solution.After shaking,the solutions were purified and enriched on an Oasis HLB SPE column.The target analytes were separated on an ACQUITY UPLC BEH C18 chromatographic column(100 mm×2.1 mm,1.7μm)at a column temperature of 40℃with a flow rate of 0.4 mL/min.The injection volume was 10μL.Gradient elution was carried out with methanol and 0.1%formic acid aqueous solution as the mobile phases.Multiple reaction monitoring(MRM)was conducted in the positive and negative electrospray ionization modes.The
机构地区 安徽省疾病预防控制中心
出处 《色谱》 CAS CSCD 北大核心 2021年第4期406-414,共9页 Chinese Journal of Chromatography
关键词 超高效液相色谱-串联质谱 固相萃取 基质效应 同位素内标 兽药残留 代谢物 动物源性食品 ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) solid phase extraction(SPE) matrix effect(ME) isotope internal standard veterinary drug residues metabolites animal-derived foods
分类号 O658 [理学—分析化学]
