一种用于分离注射用粉末制剂中异构头孢曲松的高效薄层色谱密度测定法。

A high-performance thin-layer chromatography densitometric method for the separation of isomeric ceftriaxone in powder for injection formulation.

机构信息

Pharm R&D Lab and Department of Medicinal Chemistry, School of Pharmacy, Muhimbili University of Health and Allied Sciences, P. O. Box 65545, Dar es Salaam, Tanzania.

Tanzania Medicines and Medical Devices Authority, P. O. Box 1253, Dodoma, Tanzania.

出版信息

Sci Rep. 2024 Nov 1;14(1):26308. doi: 10.1038/s41598-024-77334-5.

DOI:10.1038/s41598-024-77334-5

PMID:39487191

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11530466/

Abstract

The aim of this study was to develop and validate a High-Performance Thin Layer Chromatographic (HPTLC) method for simultaneous determination of ceftriaxone and ceftriaxone e-isomer in powder for injection formulation. Ceftriaxone sodium injection is an antibiotic that used globally. It has Z/E geometrical conformation, in which ceftriaxone sodium and 3 ene-isomer have Z- conformation while (E)-isomer has E- conformation and the potential toxicity of ceftriaxone (E)-isomer has been reported. Thus, to safeguard the public health, a simple and easy to use, rapid and reliable method was developed for qualitative and quantitative determination of ceftriaxone sodium and its (E)-isomer. Samples were applied on HPTLC glass plates precoated with silica gel 60F254 by using Linomat semi-auto sampler. Separation was carried out using acetone, triethyl amine, water, chloroform and ethyl acetate as a mobile phase in different ratios. The R values of separated compounds were 0.51 ± 0.01 and 0.62 ± 0.01 for ceftriaxone sodium and ceftriaxone (E)-isomer respectively. The method was validated by studying Specificity, Linearity, Accuracy, Precision, Robustness, Limit of Detection (LOD) and Limit of Quantification (LOQ) and Solution stability. The developed method was successfully, sensitive, simple, precise, accurate, robust and applicable for the simultaneous determination of ceftriaxone sodium and ceftriaxone (E)-isomer in powder for injection formulation.

摘要

本研究旨在开发和验证一种高效薄层色谱（HPTLC）方法，用于同时测定注射用粉体制剂中的头孢曲松和头孢曲松 E-异构体。头孢曲松钠注射液是一种在全球使用的抗生素。它具有 Z/E 几何构象，其中头孢曲松钠和 3 烯异构体具有 Z-构象，而（E）-异构体具有 E-构象，并且已经报道了头孢曲松（E）-异构体的潜在毒性。因此，为了保障公众健康，开发了一种简单易用、快速可靠的定性和定量测定头孢曲松钠及其（E）-异构体的方法。样品通过 Linomat 半自动取样器涂覆在硅胶 60F254 预涂的 HPTLC 玻璃板上。使用不同比例的丙酮、三乙胺、水、氯仿和乙酸乙酯作为流动相进行分离。分离化合物的 R 值分别为 0.51±0.01 和 0.62±0.01，分别为头孢曲松钠和头孢曲松（E）-异构体。通过研究专属性、线性、准确性、精密度、稳健性、检测限（LOD）和定量限（LOQ）以及溶液稳定性对方法进行了验证。所开发的方法成功、灵敏、简单、精确、准确、稳健，适用于注射用粉体制剂中头孢曲松钠和头孢曲松（E）-异构体的同时测定。