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首页> 外文期刊>Oriental Journal of Chemistry: An International Research Journal of Pure & Applied Chemistry >Pre-Column derivatization Chiral HPLC Method for the separation and quantification of (R,R)-2,8-diazobicyclo [4.3.0]nonane content in (S,S)-2,8-diazobicyclo[4.3.0]nonane, A Key Intermediate of Moxifloxacin Hydrochloride
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Pre-Column derivatization Chiral HPLC Method for the separation and quantification of (R,R)-2,8-diazobicyclo [4.3.0]nonane content in (S,S)-2,8-diazobicyclo[4.3.0]nonane, A Key Intermediate of Moxifloxacin Hydrochloride

机译:柱前衍生手性HPLC方法分离和定量(S,S)-2,8-二重氮双环[4.3.0]壬烷中的(R,R)-2,8-重氮二环[4.3.0]壬烷含量,盐酸莫西沙星的关键中间体

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摘要

A simple and robust analytical method was developed for the separation and quantification of (R,R)-isomer in (S,S)-2,8-diazobicyclo[4.3.0]nonane, a non chromophoric moiety and key intermediate in the synthesis of Moxifloxacin hydrochloride by using pre-column derivatization reagent 4-Chloro-7-nitrobenzofurazan (NBD Chloride). The derivatization was brought to be optimized at room temperature. The separation was achieved on Chiralpak IC 250 mm x 4.6 mm, 5 urn column with isocratic elution mode with a flow rate of 1.0 mL min~(-1). The mobile phase was a mixture of methanol, ethanol and diethyl amine in the ratio of 1:1:0.1 (v/v/v). The eluents were monitored at 340 nm using a UV detector.
机译:开发了一种简单而稳定的分析方法,用于分离和定量(S,S)-2,8-重氮二环[4.3.0]壬烷中的(R,R)-异构体,该化合物是非发色部分,是合成中的关键中间体柱前衍生试剂4-氯-7-硝基苯并呋喃酯(NBD氯化物)制备盐酸莫西沙星。使衍生化在室温下最优化。在Chiralpak IC 250 mm x 4.6 mm,5 um色谱柱上以等度洗脱模式进行分离,流速为1.0 mL min〜(-1)。流动相是比例为1:1:0.1(v / v / v)的甲醇,乙醇和二乙胺的混合物。使用UV检测器在340nm下监测洗脱液。

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