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首页> 外文期刊>Saudi Pharmaceutical Journal >Optimization of HPLC method for determination of cefixime using 2-thiophenecarboxaldehyde as derivatizing reagent: A new approach
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Optimization of HPLC method for determination of cefixime using 2-thiophenecarboxaldehyde as derivatizing reagent: A new approach

机译:以2-噻吩甲醛为衍生剂测定头孢克肟的HPLC方法的优化:一种新方法

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摘要

The determination of cefixime 1 has clinical and analytical importance due to its broad spectrum antimicrobial activity and stability. Cefixime is a significant member of orally active third generation cephalosporin and has excellent activity against many pathogens. It is for first time that we have developed a new HPLC-DAD method for analysis of imine derivative 3 of cefixime by using reflux method at 100^oC for 50min without any buffer solution. 2 Thiophenecarboxaldehyde (2TCA) 2 was used first time as a derivatizing reagent for cefixime drug. Furthermore, separation of three components, i.e. drug (cefixime), reagent (2TCA) and derivative was carried out using kromasil 100 C-18 (15mmx0.46mm, 5@mm) column with isocratic elution of methanol: 0.1% aqueous formic acid (70:30v/v) with flow rate of 1mlmin^-^1 at retention time of 1.8, 2.4 and 3.3min, respectively; while, total run time was 5min. The developed method was repeatable with a relative standard deviation (RSD) of 0.81-1.88% for imine derivative. The limit of detection and quantification of imine derivative 3 were obtained within the range of 0.132-0.401@mgml^-^1 and compared with cefixime drug as 0.30-0.90@mgml^-^1, respectively. However, the formation of imine derivative 3 was confirmed by comparing peak height, retention time and spectral changes. The method is rapid, simple, very stable and accurate for the separation and determination of imine derivative 3 of cefixime 1.
机译:头孢克肟1的测定因其广谱的抗菌活性和稳定性而具有临床和分析意义。头孢克肟是口服第三代头孢菌素的重要组成部分,对许多病原体都有极好的活性。这是我们首次开发出一种新的HPLC-DAD方法,该方法通过使用回流法在100°C下50分钟不使用任何缓冲液的情况下分析头孢克肟的亚胺衍生物3。 2噻吩甲醛(2TCA)2首次用作头孢克肟药物的衍生试剂。此外,使用kromasil 100 C-18(15mmx0.46mm,5 @ mm)色谱柱进行等度洗脱,用甲醇:0.1%甲酸水溶液( 70:30v / v),流速分别为1mlmin ^-^ 1,保留时间分别为1.8、2.4和3.3min;而总运行时间为5分钟。所开发的方法可重复使用,亚胺衍生物的相对标准偏差(RSD)为0.81-1.88%。亚胺衍生物3的检出限和定量限在0.132-0.401@mgml^-^1的范围内,与头孢克肟类药物的比较范围分别为0.30-0.90@mgml^-^1。但是,通过比较峰高,保留时间和光谱变化可以确认亚胺衍生物3的形成。该方法快速,简便,稳定,准确,可用于头孢克肟1亚胺衍生物3的分离和测定。

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