养殖废水中四环素HPLC分析方法的研究  

Research of Analytial Meathod about Tetracyclines of Wastewater in Pig Farm by HPLC

作　　者：贺蕴普[1] 贺德春[2] 王志良[3] 韩静磊[4] 徐彬[1] 

机构地区：[1]中国科学院广州化学研究所,广东广州510650 [2]湖南农业大学资源环境学院,湖南长沙410128 [3]江苏省环境科学研究院,江苏南京210036 [4]环境保护部华南环境科学研究所,广东广州510655

出　　处：《广州化学》2011年第1期26-31,共6页Guangzhou Chemistry

基　　金：江苏省环境工程重点实验室开放基金资助项目(KF200900x)

摘　　要：为了评价养殖废水中四环素类抗生素残留的状况,建立了养猪场废水中四种常见四环素类抗生素(土霉素、四环素、金霉素、强力霉素)的高效液相色谱分析方法。水样中四环素类药物经HLB固相萃取小柱吸附,甲醇乙酸乙酯溶液洗脱后用高效液相色谱紫外检测器测定。在0.05～10.00μg/mL范围内,四种抗生素的峰面积与质量浓度的线性关系良好(R2≥0.999),对土霉素、四环素、金霉素、强力霉素的最低检测质量浓度分别为0.10、0.15、0.30、0.18μg/L,当添加质量浓度为0.01μg/mL和0.1μg/mL时,四种四环素类抗生素的平均回收率分别为83.35%～93.32%和86.72%～92.46%,相对标准偏差小于8.27%。该方法分离效果好,萃取简单,速度快,可满足养殖场废水中残留四环素类抗生素的测定。6个养殖场水样测定结果表明,四种药物在养殖废水中均有检出。A method for the determination of 4 tetracyclines（TCs）（oxytetracyline,tetracycline,chlortetracycline,doxytetracyline） redidues in wastewater of pig farm was developed by high performance liquid chromatography（HPLC） with ultraviolet（UV） detector.After adsorbed with a waters oasis hydrophile-lipophile balance solid phase extraction cartridge and eluted by methanol（10%）-acetal,TCs were detected by HPLC-UV.The calibration curve was linear in the range 0.05～10.00 mg/L and R2≥0.999.The limit of quantification（LOQ） was 0.10、0.15、0.30、0.18 μg/L and the recovery rates were 83.35%～93.32% and 86.72%～92.46% with the relative standard deviation（RSD）8.27% at the spiking level 10.00 and 100.00 ng/mL,respectively,for oxytetracyline,tetracycline,chlortetracycline and doxytetracyline in wastewater.The method was suitable for the detection of TCs residues in wastewater.The four TCs were detected in wastewater sampled from six pig farms.

关 键 词：养殖废水 高效液相色谱 四环素 土霉素 金霉素 强力霉素 

分 类 号：X703[环境科学与工程—环境工程]