固相萃取-液相色谱-串联三重四极杆质谱法检测鸡蛋中6种喹诺酮类药物含量

Determination of 6 kinds of quinolone residues in eggs by solid-phase extraction combined with liquid chromatography-tandem triple quadrupole mass spectrometry

中文关键词:  喹诺酮类  液相色谱-串联三重四级杆质谱法  固相萃取  鸡蛋

英文关键词:quinolones  liquid chromatography-tandem triple quadrupole mass spectrometry  solid-phase extraction  egg

中文摘要:

      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 C18色谱柱(100 mm×2.1 mm, 1.7 μm)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1.0~100.0 μg/kg范围内线性关系良好(r2>0.999), 检出限为0.13~0.25 μg/kg, 定量限为0.43~0.83 μg/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。

英文摘要:

      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 C18 column (100 mm×2.1 mm, 1.7 μm) 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 1.0–100.0 μg/kg with correlation coefficients (r2) more than 0.999. The limits of detection and limits of quantitation were 0.13–0.25 μg/kg and 0.43–0.83 μg/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.