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[目的]建立一种固相萃取-超高效液相色谱测定饮用水中四环素类抗生素的检测方法。[方法]取200 m L水样,以10~15 m L/min的流速通过Oasis HLB固相萃取小柱,然后用甲醇和乙酸乙酯混合溶液(体积比为1∶9)洗脱,氮气吹干,以体积分数为30%的甲醇溶液定容至1.0 m L,取10μL水样采用超高效液相色谱仪进行检测。[结果]4种抗生素的线性范围为0.05~1.00 mg/L,r>0.998,方法检出限为0.063~0.250μg/L,方法的平均加标回收率为77.2%~136.0%,相对标准偏差为0.88%~5.86%。12份出厂水和末梢水均未检出目标抗生素。[结论]本方法样品前处理简便、液相色谱分析时间短、线性范围宽、检出限较低,适合检测饮用水中四环素类抗生素。
[Objective] To establish a solid phase extraction - ultra performance liquid chromatography detection of tetracycline antibiotics in drinking water. [Method] The water sample of 200 m L was passed through the Oasis HLB solid phase extraction cartridge at a flow rate of 10-15 m L / min and then eluted with a mixture of methanol and ethyl acetate (1: 9 by volume). Nitrogen Dried to a volume fraction of 30% methanol solution volume to 1.0 m L, take 10μL water samples were detected by ultra performance liquid chromatography. [Result] The linear range of the four antibiotics was 0.05-1.00 mg / L with r> 0.998. The detection limits were 0.063-0.250 μg / L. The average recoveries of the four antibiotics were 77.2% -136.0%. The relative standard deviations 0.88% ~ 5.86%. No target antibiotics were detected in 12 samples of factory water and peripheral water. [Conclusion] The method has the advantages of simple pre-treatment, short time of liquid chromatographic analysis, wide linear range and low detection limit, and is suitable for detecting tetracycline antibiotics in drinking water.