摘要
目的建立固相萃取-液相色谱-串联三重四极杆质谱法测定鸡蛋中6种喹诺酮类药物(氧氟沙星、诺氟沙星、洛美沙星、培氟沙星、恩诺沙星、环丙沙星)残留量的方法。方法鸡蛋样品经0.1 mol/L乙二胺四乙酸-麦克尔维恩(ethylenediaminetetraacetic acid-Mcllvaine,EDTA-Mcllvaine)缓冲液提取,HLB固相萃取柱净化,Acquity BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)分离,以甲醇-乙腈(4:6,V:V)和0.2%甲酸水为流动相梯度洗脱,电喷雾电离源(electrospray ionization,ESI+)正离子模式扫描,多反应监测(multiple reaction monitoring,MRM)模式下检测,基质匹配标准曲线法定量。结果6种喹诺酮类药物在1.0~100.0μg/kg范围内线性关系良好(r^(2)>0.999),检出限为0.13~0.25μg/kg,定量限为0.43~0.83μg/kg,平均回收率为94.6%~108.0%,相对标准偏差为2.48%~6.34%(n=3)。结论该方法灵敏度高、抗干扰能力强,适用于鸡蛋中喹诺酮类药物残留的快速检测,为食品安全监管提供可靠的技术支持。
Objective To establish a method for the determination of 6 kinds of quinolone residues(ofloxacin,norfloxacin,lomefloxacin,pefloxacin,enrofloxacin and ciprofloxacin)in eggs by solid-phase extraction combined with liquid chromatography-tandem triple quadrupole mass spectrometry.Methods Egg samples were extracted with 0.1 mol/L ethylenediaminetetraacetic acid-Mcllvaine(EDTA-Mcllvaine)buffer,purified by HLB solid-phase extraction cartridges and separated on an Acquity BEH C_(18) column(100 mm×2.1 mm,1.7μm)using a gradient elution with methanol-acetonitrile(4:6,V:V)and 0.2%formic acid aqueous solution as the mobile phase.The analytes were detected in positive electrospray ionization(ESI+)mode with multiple reaction monitoring(MRM),quantified using a matrix-matched calibration curve.Results The 6 kinds of quinolones exhibited good linearity in the range of 1.0–100.0μg/kg with correlation coefficients(r^(2))more than 0.999.The limits of detection and limits of quantitation were 0.13–0.25μg/kg and 0.43–0.83μg/kg,respectively.The average recoveries ranged from 94.6%to 108.0%,with relative standard deviations of 2.48%–6.34%(n=3).Conclusion The developed method is simple,sensitive and robust,suitable for the rapid detection of quinolone residues in eggs,providing technical support for food safety monitoring.
作者
吕奔阳
丁圣修
李忠春
徐婧
李伟
丁文均
包名家
刘凤海
LV Ben-Yang;DING Sheng-Xiu;LI Zhong-Chun;XU Jing;LI Wei;DING Wen-Jun;BAO Ming-Jia;LIU Feng-Hai(School of Public Health,Mudanjiang Medical University,Mudanjiang 157011,China;Mudanjiang Center for Disease Control and Prevention,Mudanjiang 157021,China;Heilongjiang Provincial Center for Disease Control and Prevention,Harbin 150030,China)
出处
《食品安全质量检测学报》
2026年第4期121-128,共8页
Journal of Food Safety and Quality
基金
黑龙江省重点研发计划项目(2025ZX05A03,2024ZX12C34)
黑龙江省省属高校基本科研业务费项目(2024-KYYWF-0491)。
关键词
喹诺酮类
液相色谱-串联三重四极杆质谱法
固相萃取法
鸡蛋
quinolones
liquid chromatography-tandem triple quadrupole mass spectrometry
solid-phase extraction
egg
