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目的建立固相萃取-超高效液相色谱-串联质谱法同时测定水中氯霉素、氟甲砜霉素和4种四环素类抗生素的检测方法。方法样品经HLB固相萃取柱富集、净化后用甲醇洗脱,以超高效液相色谱-串联质谱(UPLC-MS/MS)多反应监测(MRM)正负离子切换模式检测测定水中抗生素残留,外标法定量。结果方法的线性范围为2μg/L~200μg/L,线性相关系数0.9988~0.9995,检出限0.08 ng/L~5.21 ng/L;出厂水和水源水的平均加标回收率分别为82.3%~96.1%和80.4%~92.4%;相对标准偏差(RSD)2.6%~6.8%。结论该方法具有操作简单、干扰少、快速、准确可靠的特点,适用于水样品中抗生素残留的定量及确证检测。
OBJECTIVE To establish a method for simultaneous determination of chloramphenicol, florfenicol and four kinds of tetracycline antibiotics in water by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were enriched by HLB solid phase extraction (SPE) column and eluted with methanol after purification. The residues of antibiotics in water were detected by UPLC-MS / MS MRM mode. External standard method. Results The linear range of the method was 2μg / L ~ 200μg / L with a linear correlation coefficient of 0.9988 ~ 0.9995 and a limit of detection of 0.08 ng / L ~ 5.21 ng / L. The average spike recoveries of effluent and tap water were 82.3% 96.1% and 80.4% -92.4%, respectively. The relative standard deviations (RSDs) ranged from 2.6% to 6.8%. Conclusion The method has the advantages of simple operation, less interference, fast, accurate and reliable. It is suitable for the quantitative and confirmatory testing of antibiotic residues in water samples.