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首页> 外文期刊>Atomic Spectroscopy >Ion pair solid phase extraction for the indirect determination of gatifloxacin by flow injection flame atomic absorption spectrometry
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Ion pair solid phase extraction for the indirect determination of gatifloxacin by flow injection flame atomic absorption spectrometry

机译:离子对固相萃取-流动注射火焰原子吸收光谱法间接测定加替沙星

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A flow injection flame atomic absorption spectrometry (FAAS) method with on-line ion pair solid-phase extraction was developed for the indirect determination of gatifloxacin. In a flow injection system, gatifloxacin reacted first with Fe(III) to form a 2:1 complex cation, then the cation reacted with ClO4- to form a neutral ion pair complex of gatifloxacin-Fe(III)-ClO4 and was adsorbed on a C-18 solid phase extraction column, while excessive Fe(III) was washed with H2O to waste. The ion pair complex adsorbed was eluted with a mixture of ethanol, water, and acetonitrile (48:32:20, v/v/v), Fe(III) in t e comp ex was an determined with FAAS. The optimization of various experimental conditions was investigated. With a reaction and extraction time of 60 seconds, the calibration curve was linear, ranging from 0.05 to 12.50 mu g mL(-1) with a relative standard deviation of 2.0% (n = 11, c = 5.0 mu g mL(-1) and the detection limit for gati floxacin was 0.02 mu g mL(-1). The analytical frequency was 24 samples per hour. The method was validated by the determination of gatifloxacin in capsules and tablets, and the recoveries obtained were 95-106%. This procedure not only provides a sensitive analytical method for gatifloxacin determination, but also offers a new approach for the application of FAAS in the indirect determination of organic species.
机译:建立了在线离子对固相萃取的流动注射火焰原子吸收光谱法(FAAS),用于间接测定加替沙星。在流动注射系统中,加替沙星首先与Fe(III)反应形成2:1配位阳离子,然后阳离子与ClO4-反应形成加替沙星-Fe(III)-ClO4的中性离子对配合物,并被吸附在C-18固相萃取柱,而过量的Fe(III)用H2O洗涤以浪费。吸附的离子对络合物用乙醇,水和乙腈的混合物(48:32:20,v / v / v)洗脱,用FAAS测定化合物中的Fe(III)。研究了各种实验条件的优化。反应和提取时间为60秒,校准曲线呈线性,范围为0.05至12.50μg mL(-1),相对标准偏差为2.0%(n = 11,c = 5.0μg mL(-1) ),加替沙星的检出限为0.02μg mL(-1),分析频率为每小时24个样品,通过测定胶囊和片剂中加替沙星的方法验证了该方法的有效性,回收率为95-106%该方法不仅为加替沙星的测定提供了灵敏的分析方法,而且为FAAS在间接测定有机物中的应用提供了一种新方法。

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