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固相萃取-液质联用法同时测定水中的喹诺酮类和磺胺类抗生素 被引量:16

Simultaneous Determination of Quinolones and Sulfonamides in Water Samples by Solid Phase Extraction-Ultra Performance Liquid Chromatography Electrospray Tandem Mass Spectrometry
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摘要 建立了固相萃取-超高效液相色谱三重四级杆质谱联用法同时测定水中痕量的5种喹诺酮类和6种磺胺类抗生素残留的方法,水样经过固相萃取富集后由液相色谱分离、三重四级杆质谱检测。该方法在8 min内完成对11种目标化合物的分析。喹诺酮类抗生素线性范围为0.5~50μg/L,磺胺类抗生素线性范围为1~100μg/L,相关系数均大于0.995,6次空白加标重复测定的相对标准偏差(n=6)为喹诺酮类抗生素5.3%~9.0%,磺胺类抗生素4.7%~10.2%。11种目标化合物的方法检出限在0.04~0.22 ng/L之间,实际样品的加标回收率为62.1%~137%。该方法操作简便,重现性好,可用于地表水中抗生素的检测。 A rapid analytical method for simultaneous determination of five quinolones(QNs) and six sulfonamides(SAs) in water sample was developed. Water samples were purified and concentrated by solid phase extraction (SPE) then analyzed by ultra performance liquid chromatography electrospray tandem mass spectrometry (UPLC-MS / MS). The analysis of QNs and SAs can be finished in 8 minutes. The linear ranges were 0.5-50 μg/L for quinolones and 1-100 μg/L for sulfonamides, respectively. All the correlation coefficients were more than 0.995. The relative standard deviations of spiked blank samples (n=6) were 5.3%-9.0% for quinolones and 4.7%-10.2% for sulfonamides, respectively. The limits of determination for analytes were in the range of 0.04-0.22 ng/L. The average recovery rate of real samples was in the range of 62.1%,137%. This method is simple and has good repeatability, it is suitable for determination of QNs and SAs in water sample.
出处 《化学分析计量》 CAS 2013年第3期29-32,共4页 Chemical Analysis And Meterage
基金 江苏省环境监测基金项目(1006)
关键词 喹诺酮类 磺胺类 液质联用 固相萃取 quinolone sulfonamide UPLC-MS/MS SPE
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