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间接分光光度法测定头孢曲松钠:基于铜(II)在正丙醇 - 硫酸铵 - 水体系中的萃取浮选

Indirect spectrophotometric determination of sodium ceftriaxone with n-propyl alcohol-ammonium sulfate-water system by extraction flotation of copper(II).

作者信息

Zhao Wei, Zhang Yan, Li Quanmin

机构信息

College of Chemistry and Environmental Science, Henan Normal University, The Key Laboratory of Environmental Pollution Control Technology of Henan, Xinxiang, Henan, PR China.

出版信息

Clin Chim Acta. 2008 May;391(1-2):80-4. doi: 10.1016/j.cca.2008.02.010. Epub 2008 Feb 16.

Abstract

BACKGROUND

Although the determination methods of sodium ceftriaxone has been increasingly reported, these methods have their inherent limits preventing them from being broadly applied in common laboratories. In order to circumvent this problem, a rapid and simple method for the indirect spectrophotometric determination of sodium ceftriaxone is reported.

METHOD

Sodium ceftriaxone was degraded completely in the presence of 0.20 mol/l sodium hydroxide in boiling water bath for 20 min. The thiol group (-SH) of the degradation product (I) of sodium ceftriaxone could reduce cupric to cuprous ions, and the resulting which was precipitated with the thiol group (-SH) of the degradation product (II) at pH 4.0. By determining the residual amount of copper (II), the indirect determination of sodium ceftriaxone can be achieved.

RESULT

Standard curve of sodium ceftriaxone versus the flotation yield of copper(II) showed that sodium ceftriaxone could be determined in low concentrations. The linear range of sodium ceftriaxone was 0.70-32 microg/ml and the detection limit evaluated by calibration curve (3sigma/k) was found to be 0.60 microg/ml.

CONCLUSION

A simple and efficient method was developed and it has been successfully applied to the determination of sodium ceftriaxone in human serum and urine samples, respectively. It is expected that this method will find broad applications in the detection of cephalosporin derivatives with similar structure.

摘要

背景

尽管头孢曲松钠的测定方法报道日益增多,但这些方法存在固有局限性,阻碍其在普通实验室广泛应用。为解决此问题,报道了一种间接分光光度法快速简便测定头孢曲松钠的方法。

方法

头孢曲松钠在0.20 mol/l氢氧化钠存在下于沸水浴中完全降解20分钟。头孢曲松钠降解产物(I)的巯基(-SH)可将铜离子还原为亚铜离子,所得产物在pH 4.0时与降解产物(II)的巯基(-SH)沉淀。通过测定铜(II)的残留量,可间接测定头孢曲松钠。

结果

头孢曲松钠与铜(II)浮选产率的标准曲线表明,低浓度下可测定头孢曲松钠。头孢曲松钠的线性范围为0.70 - 32 μg/ml,通过校准曲线(3σ/k)评估的检测限为0.60 μg/ml。

结论

开发了一种简单有效的方法,已成功分别应用于人体血清和尿液样本中头孢曲松钠的测定。预计该方法将在检测具有类似结构的头孢菌素衍生物中得到广泛应用。

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