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Simultaneous determination of nitroimidazoles and amphenicol antibiotics in water samples using ultrasound-assisted dispersive liquid-liquid microextraction coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry

机译:超声辅助分散液-液微萃取-超高效液相色谱-串联质谱法同时测定水样中的硝基咪唑和氨苄类抗生素

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摘要

A rapid, simple and environmentally friendly method involving ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) was developed for the simultaneous determination of nitroimidazoles (metronidazole and tinidazole) and amphenicol antibiotics (chloramphenicol and thiamphenicol) in water samples. In this work, the effective DLLME parameters such as pH, the type and volume of extraction solvent, the type and volume of dispersive solvent, salt concentration and extraction time were investigated. The significant factors were optimized and selected as follows: pH 4.0 water sample, 300 mu L dichloromethane, 600 mu L acetonitrile, no salt addition and 4 min of extraction time. Under the optimum conditions, the calibration curves were linear in the range of 2.00-100 ng L-1 (MNZ and TNZ) and 5.00-200 ng L-1(CAP and TAP) with regression coefficients (r) higher than 0.9917. Limits of detection (LODs) and limits of quantification (LOQs) were achieved in the range of 0.39-1.38 ng L-1 and 1.70-4.18 ng L-1, respectively. The relative recoveries of the analytes were from 82.8% to 99.5% with the relative standard deviations between 0.3% and 4.3%. The developed method was successfully applied to analyze the nitroimidazoles and amphenicol antibiotics in water samples with satisfactory results.
机译:建立了一种超声辅助分散液-液微萃取(UA-DLLME)结合超高效液相色谱-串联质谱(UHPLC-MS / MS)的快速,简单,环保方法,用于同时测定硝基咪唑的方法(甲硝唑和替硝唑)和安非他汀类抗生素(氯霉素和甲砜霉素)在水样中的含量。在这项工作中,研究了DLLME的有效参数,例如pH,萃取溶剂的类型和体积,分散溶剂的类型和体积,盐浓度和萃取时间。优化并选择以下重要因素:pH 4.0的水样品,300μL的二氯甲烷,600μL的乙腈,不添加盐和4分钟的萃取时间。在最佳条件下,校正曲线在2.00-100 ng L-1(MNZ和TNZ)和5.00-200 ng L-1(CAP和TAP)之间呈线性,回归系数(r)大于0.9917。检测限(LOD)和定量限(LOQ)分别达到0.39-1.38 ng L-1和1.70-4.18 ng L-1。分析物的相对回收率从82.8%到99.5%,相对标准偏差在0.3%和4.3%之间。该方法成功用于水样中的硝基咪唑类和氨苄类抗生素的分析,结果令人满意。

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