高效液相色谱法同时测定水产品中6 种喹诺酮药物的残留

建立用固相萃取- 反相高效液相色谱法同时检测水产品中6 种喹诺酮药物残留量的方法。通过对提取方法和C18 固相萃取柱净化条件、色谱条件选择与优化、洗脱液浓度和用量的选择方面的研究，确定采用高效液相色谱分离、荧光检测器检测、外标法定量的分析方法。本方法对环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹标准曲线的线性回归系数均在0.99 以上，线性范围为0.02～2.0μg/mL。以3 倍信噪比RSN 计算，环丙沙星、恩诺沙星、诺氟沙星、氧氟沙星检出限为2μg/kg，噁喹酸、氟甲喹检出限为5μg/kg；以10 倍信噪比RSN 计算，环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星的定量下限为5μg/kg；噁喹酸、氟甲喹的定量下限为10μg/kg。在南美白对虾、罗非鱼、鳗鱼、斑点叉尾鮰中进行这6 种喹诺酮类药物加标回收率的验证实验，实验结果满意，回收率在78.8%～92.9% 之间；相对标准偏差为2.97%～7.10%。说明本方法简单、灵敏，结果可靠，可用于水产品中环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹的同时检测。

High Performance Liquid Chromatographic Method for Simultaneous Determination of Six Quinolone Residues in Aquatic Products

A solid-phase extraction followed by reversed-phase high performance liquid chromatographic (SPE-RP-HPLC) method was presented for the simultaneous determination of 6 quinolone residues (enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin, oxolinic acid and flumequine) in aquatic products. Sample extraction, cleanup on a C18 cartilage column and chromatographic separation were investigated. A RP-HPLC system equipped with fluorescence detector (λex = 280 nm, λem = 480 nm) was used for analyzing 6 quinolones, and their quantification was achieved by external standard method. Six quinolones exhibited good linearity within the range of 0.02－2.0 μg/mL and the regression coefficients were all over 0.99. The developed method showed limits of detection of 2 μg/kg for ciprofloxacin, enrofloxacin, norfloxacin, ofloxacin and 5 μg/kg for oxolinic acidand flumequine (RSN = 3), and limits of quantification of 5 μg/kg for ciprofloxacin, enrofloxacin, norfloxacin, ofloxacin and 10μg/kg for oxolinic acid and flumequine (RSN = 10). Satisfying results were obtained in spike recovery experiments and average spike recoveries of 5 replicates at three levels were within the range of 78.8%－92.9%, with RSD range of 2.97%－7.10%. This method, thanks to its simplicity, sensitivity and reliability, has good suitability for the simultaneous determination of 6 quinolone residues in aquatic products.