Tan Jianhu, Tang Caiming, Yu Yiyi, Peng Xianzhi
State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China.
Se Pu. 2007 Jul;25(4):546-9.
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.
开发了一种简单可靠的方法,用于同时测定水环境中的多类抗生素残留,包括三种氟喹诺酮类药物(氧氟沙星、诺氟沙星、环丙沙星)、三种磺胺类药物(磺胺嘧啶、磺胺甲恶唑、磺胺二甲嘧啶)、氯霉素和甲氧苄啶。样品通过亲水亲脂平衡(HLB)柱进行萃取和浓缩。采用内标定量法,通过高效液相色谱(HPLC)测定选定的抗生素化合物。抗生素在安捷伦XRD C18柱(150 mm×3.0 mm,3.5μm)上分离,使用乙腈和0.1%(v/v)甲酸的纯化水进行梯度洗脱,流速为0.25 mL/min,柱温为25℃。氟喹诺酮类药物通过荧光检测(FLD)定量,其他药物通过280 nm的紫外检测定量。加标自来水的抗生素回收率分别为80%至120%,城市河水样品的回收率为63%至106%,相对标准偏差低于18%。地表水的定量限为0.030 - 0.080μg/L。该方法已成功应用于监测广州珠江城市河水中抗生素残留的情况。检测到磺胺甲恶唑、氧氟沙星、诺氟沙星和环丙沙星的质量浓度范围为0.197至0.510μg/L。