高效液相色谱法同时分析城市河水中的多种抗生素

结合固相萃取（SPE）与高效液相色谱（HPLC）分析,建立了一种适用于我国城市水环境中多种抗生素的分析方法,同时分析城市水体中3种磺胺类(磺胺嘧啶、磺胺甲唑和磺胺二甲基嘧啶)、3种喹诺酮类(氧氟沙星、诺氟沙星和环丙沙星)、氯霉素以及甲氧苄氨嘧啶等8种抗生素污染物。水样品由稀盐酸调节pH值后经HLB固相萃取小柱萃取,用内标法通过HPLC定量分析上述抗生素污染物。采用Agilent Zorbax Eclipse XRD C18液相色谱柱(150 mm×3.0 mm,3.5 μm),用乙腈-水(含0.1%甲酸)二元流动相进行梯度洗脱，流速为0.25 mL/min,柱温25 ℃。喹诺酮类抗生素使用荧光检测器(FLD)定量,其他抗生素则采用紫外检测器定量。该方法对自来水加标的回收率为80%～120%,对地表水样品加标的回收率为63%～106%,方法的定量检测限为0.030～0.080 μg/L,相对标准偏差小于18%。利用该方法对珠江广州河段的水体进行了分析,检测到磺胺甲唑、氧氟沙星、诺氟沙星及环丙沙星,质量浓度范围为0.197～0.510 μg/L。

Simultaneous Analysis of Multiple Classes of Antibiotics in Urban River Water by High Performance Liquid Chromatography

A simple and reliable method was developed for simultaneous determination of multi-class antibiotic residues in aquatic environment, including three fluoroquinolones (ofloxacin, norfloxacin, ciprofloxacin), three sulfonamides (sulfadiazine, sulfamethoxazole, sulfamethazine), chloramphenicol and trimethoprim. Samples were extracted and concentrated through hydrophilic-lipophilic balance (HLB) cartridges. Selected antibiotic compounds were determined by high performance liquid chromatography (HPLC) using internal standard quantification method. Antibiotics were separated on an Agilent XRD C18 column (150 mm x 3.0 mm, 3.5 microm) with a gradient elution using acetonitrile and 0.1% (v/v) formic acid in purified water at a flow rate of 0.25 mL/min and the column temperature of 25 degree C. Fluoroquinolones were quantified by fluorescence detection (FLD) and the others by ultraviolet detection at 280 nm. The recoveries for the antibiotics are ranging from 80% to 120% for spiked tap water, and 63% to 106% for urban river water samples, respectively, with relative standard deviation lower than 18%. The limits of quantification were 0.030-0.080 microg/L for surface waters. The method has been successfully applied to monitor the occurrence of antibiotic residues in the urban river waters from the Pearl River in Guangzhou. Sulfamethoxazole, ofloxacin, norfloxacin and ciprofloxacin were detected at mass concentrations ranging from 0.197 to 0.510 microg/L.