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建立了固相萃取-高效液相色谱法同时检测废水中喹乙醇、土霉素（OTC）、四环素（TC）和金霉素（CTC）的分析方法。实验对前处理方法和色谱条件进行了探讨和优化，结果表明水样pH值为2.5，不加提取剂时OasisHLB柱的纯化富集效果最好，液相色谱在375nm处对四种物质的分离性能最佳。该方法具有良好的线性关系（r〉0.999），最低检出限为11～26ug／L。喹乙醇和3种四环素类抗生素的加标回收率分别为91％～95％，90％～91％，86％～90％和81％～86％，相对标准偏差为3．4％～6．3％。“,”An analytic method was developed for determination of olaquindox, oxytetracycline （ OTC ） , tetracycline （ TC ） and chlortrtracycline（CTC） in wastewater using solid phase extraction with high performance liquid chromatography detection. The pretreatment methods and chromatographic condition have been optimized. The optimized condition was no extractor, water sample pH 2. 5 and detective wavelength 375nm. This method had good linearity （ r 〉 0.999）, and the limits of quantification were between 11 ～ 26 ug/L. The range of recoveries for olaquindox and three tetracycline antibiotics in water sample were 91% ～ 95% ,90% ～91% ,86%～90% ,81%～ 86% with a relative standard deviation of 3.4% ～ 6.3 % respectively.