首页> 外文期刊>Journal of AOAC International >Spectrophotometric, difference spectroscopic, and high-performance liquid chromatographic methods for the determination of cefixime in pharmaceutical formulations
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Spectrophotometric, difference spectroscopic, and high-performance liquid chromatographic methods for the determination of cefixime in pharmaceutical formulations

机译:分光光度法,差示光谱法和高效液相色谱法测定药物制剂中的头孢克肟

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Three simple and sensitive spectrophotometric, difference spectroscopic, and liquid chromatographic (LC) methods are described for the determination of cefixime. The first method is based on the oxidative coupling reaction of cefixime with 3-methyl-2-benzothiazolinon hydrazone HCI in presence of ferric chloride. The absorbance of reaction product was measured at the maximum absorbance wavelength (wavelength(max)), 630 nm. The difference spectroscopic method is based on the measurement of absorbance of cefixime at the absorbance maximum, 268 nm, and minimum, 237 nm. The measured value was the amplitude of maxima and minima between 2 equimolar solutions of the analyte in different chemical forms, which exhibited different spectral characteristics. The conditions were optimized, and Beer's law was obeyed for cefixime at 1 to 16 microg/mL and 10 to 50 microg/mL, respectively. The third method, high-performance LC, was developed for the determination of cefixime using 50 mM potassium dihydrogen phosphate (pH 3.0)-methanol (78 + 22, v/v) as the mobile phase and measuring the response at wavelength(max) 286 nm. The analysis was performed on a Lichrospher RPC18 column. The calibration curve was obtained for cefixime at 5 to 250 microg/mL, and the mean recovery was 99.71 +/- 0.01%. The methods were validated according to the guidelines of the U.S. Pharmacopoeia and also assessed by applying the standard addition technique. The results obtained in the analysis of dosage forms agreed well with the contents stated on the labels.
机译:描述了三种简单灵敏的分光光度法,差示光谱法和液相色谱(LC)方法测定头孢克肟的含量。第一种方法是基于头孢克肟与3-甲基-2-苯并噻唑啉酮盐酸盐在氯化铁存在下的氧化偶联反应。在最大吸收波长(波长(最大))630 nm下测量反应产物的吸收。差异光谱法基于在最大吸光度268 nm和最小吸光度237 nm处测量头孢克肟的吸光度。测量值是不同化学形式的分析物在两种等摩尔溶液之间的最大和最小振幅,表现出不同的光谱特征。优化条件,并遵守比尔定律,头孢克肟的浓度分别为1至16微克/毫升和10至50微克/毫升。开发了第三种方法-高效液相色谱法,以50 mM磷酸二氢钾(pH 3.0)-甲醇(78 + 22,v / v)作为流动相并测量在波长(max)下的响应来测定头孢克肟286海里分析在Lichrospher RPC18色谱柱上进行。获得的头孢克肟的校准曲线为5至250微克/毫升,平均回收率为99.71 +/- 0.01%。该方法已根据美国药典的指南进行了验证,并通过应用标准添加技术进行了评估。剂型分析中获得的结果与标签上注明的内容非常吻合。

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