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简单、快速、可靠的 CE 法同时测定人尿中的环丙沙星和氧氟沙星。

Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine.

机构信息

Department of Environmental Chemistry, Faculty of Chemistry, University of Lodz, Pomorska 163, 90-236, Lodz, Poland.

Doctoral School of Exact and Natural Sciences, University of Lodz, Banacha 12/16, 90-237, Lodz, Poland.

出版信息

Sci Rep. 2022 May 11;12(1):7729. doi: 10.1038/s41598-022-11747-y.

Abstract

A simple, fast, and accurate capillary zone electrophoresis method has been developed for the determination of ciprofloxacin and ofloxacin. This method uses liquid-liquid extraction. Therefore, it is characterized by a very simple procedure of sample preparation but at the same time satisfactory precision and accuracy. The extraction process of the same urine sample was repeated three times. The extraction protocol was performed each time for 15 min with 1 mL of dichloromethane and chloroform mixture in a 3:1 volume ratio. A 0.1 mol/L phosphate-borate buffer (pH 8.40) was selected as the background electrolyte. UV detection was performed at 288 nm. The separation was carried out at a voltage of 16 kV, at a temperature of 25 °C. Experimentally evaluated LOQ values for ciprofloxacin and ofloxacin were 0.2 nmol/mL urine and 0.05 nmol/mL urine, respectively. For both analytes the calibration curves exhibited linearity over the entire tested concentration range of 1-6 nmol/mL urine. The precision of the method did not exceed 15%, and the recovery was in the range of 85-115%. The developed and validated procedure was applied to analyze human urine for the content of ciprofloxacin and ofloxacin.

摘要

已开发出一种简单、快速且准确的毛细管区带电泳法,用于测定环丙沙星和氧氟沙星。该方法采用液-液萃取。因此,它具有非常简单的样品制备程序,但同时具有令人满意的精密度和准确度。对相同的尿样进行了三次重复的萃取过程。每次萃取协议都用 1 毫升体积比为 3:1 的二氯甲烷和三氯甲烷混合物进行 15 分钟。选择 0.1mol/L 磷酸硼酸盐缓冲液(pH 8.40)作为背景电解质。在 288nm 处进行 UV 检测。在 16kV 的电压下,在 25°C 的温度下进行分离。实验评估的环丙沙星和氧氟沙星的 LOQ 值分别为 0.2nmol/mL 尿和 0.05nmol/mL 尿。对于这两种分析物,校准曲线在整个测试浓度范围内(1-6nmol/mL 尿)均表现出线性。方法的精密度不超过 15%,回收率在 85-115%范围内。所开发和验证的程序已应用于分析人尿中环丙沙星和氧氟沙星的含量。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/10ca/9095712/7d143b84e670/41598_2022_11747_Fig1_HTML.jpg

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