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A sensitive micellar liquid chromatographic method for the rectification of enantiomers of esmolol, and determination of absolute configuration and elution order
Journal of Liquid Chromatography & Related Technologies ( IF 1.0 ) Pub Date : 2020-07-31 , DOI: 10.1080/10826076.2020.1798250
Vijay Alwera 1 , Suman Sehlangia 2 , Shiv Alwera 1, 3
Affiliation  

Abstract A green chromatographic method is proposed for the enantioseparation of Esmolol (Amino alcohol) in which aqueous solution of the mixed surfactants is used as the alternative of organic solvents. In this work, the diastereomeric derivatives of racemic esmolol were prepared, under microwave heating conditions, using highly reactive activated chiral esters of the (S)-levofloxacin, (S)-ketoprofen, and (S)-ibuprofen. The prepared diastereomeric derivatives were separated using surfactant based mobile phase on RP-HPLC. The effect of the varying concentration of surfactant (Brij-35 and SDS) in the eluting phase was investigated for separation and elution of synthesized diastereomeric derivatives. The green assessment score was calculated (obtain score points were 82) for developed method. In addition, the density functional theory calculations were performed, using Gaussian 09 rev. A.02 and hybrid density functional B3LYP with 6-31 G* basis set program, in order to develop lowest energy optimized structures of diastereomeric derivatives. The optimized structures used to predict elution order of synthesized diastereomeric derivatives. Our method was characterized by the following validation parameter: LOD (0.289 ng mL−1), LOQ (0.867 ng mL−1), calibration range (0.006–6.0 mg mL−1), correlation coefficient (0.999) and recovery (99.97 and 99.85% for intra-day assay and 99.42 and 99.75% for inter-day assay). Graphical Abstract Work highlights Organic eluent free chromatographic method for determination of enantiopurity of Esmolol is proposed. Synthesis of diastereomeric derivatives of racemic amino acids with activated esters, and their enhanced separation and detection using low cost, low toxicity and efficient Micellar Liquid Chromatography (RP-HPLC). There have been developed “Lowest energy minimizing structures” of all synthesized diastereomeric derivatives used to determine elution order and elution mechanism. The method was successful in providing very low LOD and LOQ values better resolution, low retention times, and better separation factors (α) for the prepared diastereomeric derivatives of amino acids. This method has potential for application in routine analysis of esmolol in different pharmaceuticals.

中文翻译:

一种用于精馏艾司洛尔对映体的灵敏胶束液相色谱方法,并确定绝对构型和洗脱顺序

摘要 提出了一种以混合表面活性剂的水溶液代替有机溶剂的艾司洛尔(氨基醇)对映体分离的绿色色谱方法。在这项工作中,在微波加热条件下,使用 (S)-左氧氟沙星、(S)-酮洛芬和 (S)-布洛芬的高活性活化手性酯制备了外消旋艾司洛尔的非对映异构衍生物。在 RP-HPLC 上使用基于表面活性剂的流动相分离制备的非对映异构衍生物。研究了洗脱相中不同浓度的表面活性剂(Brij-35 和 SDS)对合成非对映体衍生物的分离和洗脱的影响。为开发的方法计算绿色评估分数(获得分数为 82)。此外,使用 Gaussian 09 rev 进行密度泛函理论计算。A.02 和具有 6-31 G* 基组程序的混合密度泛函 B3LYP,以开发非对映异构衍生物的最低能量优化结构。用于预测合成的非对映异构衍生物的洗脱顺序的优化结构。我们的方法的特征在于以下验证参数:LOD (0.289 ng mL-1)、LOQ (0.867 ng mL-1)、校准范围 (0.006–6.0 mg mL-1)、相关系数 (0.999) 和回收率 (99.97 和99.85% 用于日内检测,99.42 和 99.75% 用于日间检测)。图形摘要 工作亮点 提出了测定艾司洛尔对映纯度的无有机洗脱剂色谱法。外消旋氨基酸与活化酯的非对映异构衍生物的合成,及其使用低成本、低毒性和高效的胶束液相色谱 (RP-HPLC) 增强分离和检测。已经开发出所有合成的非对映异构衍生物的“最低能量最小化结构”,用于确定洗脱顺序和洗脱机制。该方法成功地为制备的氨基酸非对映异构衍生物提供了非常低的 LOD 和 LOQ 值、更好的分辨率、更低的保留时间和更好的分离因子 (α)。该方法在不同药物中艾司洛尔的常规分析中具有应用潜力。已经开发出所有合成的非对映异构衍生物的“最低能量最小化结构”,用于确定洗脱顺序和洗脱机制。该方法成功地为制备的氨基酸非对映异构衍生物提供了非常低的 LOD 和 LOQ 值、更好的分辨率、更低的保留时间和更好的分离因子 (α)。该方法在不同药物中艾司洛尔的常规分析中具有应用潜力。已经开发出所有合成的非对映异构衍生物的“最低能量最小化结构”,用于确定洗脱顺序和洗脱机制。该方法成功地为制备的氨基酸非对映异构衍生物提供了非常低的 LOD 和 LOQ 值、更好的分辨率、更低的保留时间和更好的分离因子 (α)。该方法在不同药物中艾司洛尔的常规分析中具有应用潜力。
更新日期:2020-07-31
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