固相萃取-色谱测定水、沉积物及土壤中氯霉素和3种四环素类抗生素

Determination of Chloramphenicol and Three Tetracyclines by Solid Phase Extraction and High Performance Liquid Chromatography-Ultraviolet Detection

建立了固相萃取-高效液相色谱(UV)检测水、沉积物和土壤中的氯霉素、土霉素、四环素和金霉素4种抗生素的方法。水样、土壤和沉积物样品的前处理采用EDTA-McIlvaine缓冲溶液提取,用SAX-HLB串联小柱纯化和富集,用丙酮(含10%甲醇)洗脱进一步减小天然有机质的影响。采用乙腈和0.01mol/L草酸溶液作为流动相,8min内分离4种抗生素。测定了贵阳市阿哈湖、南明河和乌江渡水库的水样及沉积物,均有抗生素检出。

A method for determination of chloramphenicol, oxytetracycline, tetracycline and chlortetracycline in water, sediment and soil, using solid phase extraction with high performance liquid chromatography-UV detection was developed. The four antibiotics in water, sediment and soil were extracted using a mixture of EDTA and Mcllvaine buffer （citric acid and sodium orthophosphate）, then cleaned-up and pre-concentrated by a tandem method using strong anion exchanger （SAX） cartridge and hydrophilic-liphophilic balance （HLB） cartridge and then eluted by acetone （including 10% methanol） to depress the interference of nature organic compounds. Using acetonitrile and 0.01 mol/L oxalic acid as the mobile phase, the four antibiotics were separated within 8 min. This method was applied to the analysis of antibiotics in lake water, fiver water and lake sediment.