通过式固相萃取超高效液相色谱串联质谱测定水产品中兽药残留  

Determination of Veterinary Drug Residues in Aquatic Products by Ultra-high Performance Liquid Chromatography by Tandem Mass Spectrometry

作　　者：张翀宇 王展华 施贝 赵超群 朱蕾颖 金绍强 梁晶晶 ZHANG Chong-yu;WANG Zhan-hua;SHI Bei(Zhejiang Institute of Food and Drug Control/Key Laboratory of Functional Food Nu-trition and Quality Safety for State Market Regulation/Key Laboratory of Health Food Quality Safety of Provincial Market Regulation,Hang-zhou,Zhejiang 310052)

机构地区：[1]浙江省食品药品检验研究院/国家市场监管重点实验室(功能食品质量与安全领域)/浙江省市场局重点实验室(保健品质量安全重点实验室),浙江杭州310052

出　　处：《安徽农业科学》2025年第5期161-164,共4页Journal of Anhui Agricultural Sciences

基　　金：浙江省市场监督管理局雏鹰计划核心项目(CY2022227)。

摘　　要：[目的]采用通过式固相萃取超高效液相色谱串联质谱法,对水产品中的兽药残留进行检测。[方法]对样品进行80%乙腈提取,利用OasisPRiMEHLB固相萃取小柱对提取液进行富集净化,采用0.1%甲酸水-乙腈溶液作为流动相进行梯度洗脱。运用串联质谱电喷雾正、负离子扫描模式,结合质谱多反应监测(MRM)模式进行分段扫描,并通过外标法进行定量分析。[结果]10种兽药残留在10~200 ng/mL线性关系良好(R2>0.99)。方法的检出限为0.24~4.07μg/kg,定量限为0.07~1.22μg/kg。在10、50、100μg/kg的加标浓度下,回收率为80.64%~117.52%,相对标准偏差(RSD)为1.3%~6.6%。[结论]该研究构建的兽药残留检测方法具有前处理简便、净化效能显著、灵敏度高等优势,可以满足动物源性食品中兽药残留的检测需求。[Objective]To detect veterinary drug residues in aquatic products by using the formula solid phase extraction-ultra high perform-ance liquid chromatography tandem mass spectrometry.[Method]After 80%acetonitrile extraction using Oasis PRiME HLB solid phase extrac-tion column enrichment purification and isolated components,0.1%formic acid water-acetonitrile solution in the mobile phase proportional gradient elution,in series mass spectrum electrospray positive and negative ion scanning mode,using mass spectrometry multi-reaction monito-ring(multiple reaction monitoring,MRM)mode segment scanning,quantified by external standard method.[Result]The 10 veterinary drug residues showed good linear relationship between 10 and 200 ng/mL(R2>0.99),the detection limit of method was 0.24-4.07μg/kg,the limit of quantification was 0.07-1.22μg/kg.At spiked concentrations of 10,50,and 100μg/kg,the recovery rate was 80.64%-117.52%,the relative standard deviation(RSD)was 1.3%-6.6%.[Conclusion]The method for detecting veterinary drug residues constructed in this study has the advantages of simple pretreatment,significant purification efficiency and high sensitivity,which can meet the detection needs of veterinary drug residues in animal derived foods.

关 键 词：兽药残留 超高效液相色谱串联质谱法 水产品 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]