A Validated Chiral Chromatography Method for Enantiomeric Separation of Pomalidomide in Human Plasma.

IF 1.5 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS Journal of chromatographic science Pub Date : 2024-08-20 DOI:10.1093/chromsci/bmae026

Gyan Vardhan, Vikas Kumar, Puran Lal Sahu, Anuj Prakash, Ramasare Prasad, Shailendra Handu, Uttam Kumar Nath, Puneet Dhamija

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Abstract

In the present work, new chiral stationary phase high-performance liquid chromatography (CSP-HPLC) method was established and validated for the quantification of pomalidomide (PMD) enantiomers in human plasma. The chromatographic enantiomeric separation was achieved on a Daicel-CSP, Chiralpack IA 4.6 × 250 mm, 5 μm; because of its advantages of high degree of retention, high resolution capacity, better reproducibility, ability to produce lower back pressure and low degree of tailing. The mobile phase was maintained as methanol: glacial acetic acid (499.50 ml:50 μL). Ultraviolet wavelength for detection was 220 nm. PMD enantiomer-I and enantiomer-II were separated at 8.83 and 15.34 min, respectively. Limit of detection and limit of quantification for each enantiomer and the calibration curve of standard PMD was linear in range between 10-5,000 ng mL-1. The method was validated according to The International Council for Harmonisation of Technical Requirements of Pharmaceuticals for Human Use (ICH(Q2R1)) specific guidelines. We found no interference peak with PMD chromatogram obtained. This is a simple, reliable and specific method for detection and quantification of enantiomer of PMD in human plasma sample.

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用于分离人血浆中泊马度胺对映体的经过验证的手性色谱法

本研究建立并验证了手性固定相高效液相色谱（CSP-HPLC）定量检测人血浆中泊马度胺（PMD）对映体的新方法。采用 Daicel-CSP, Chiralpack IA 4.6 × 250 mm, 5 μm色谱柱进行对映体分离；该色谱柱具有保留度高、分辨能力强、重现性好、背压低、尾气少等优点。流动相为甲醇：冰醋酸（499.50 ml:50 μL）。紫外检测波长为 220 nm。PMD 对映体-I 和对映体-II 的分离时间分别为 8.83 分钟和 15.34 分钟。每种对映体的检出限和定量限以及标准 PMD 的校准曲线在 10-5,000 ng mL-1 范围内呈线性关系。该方法根据国际人用药品技术要求协调理事会（ICH(Q2R1)）的指导原则进行了验证。我们发现所获得的 PMD 色谱图没有干扰峰。该方法简便、可靠、特异，可用于检测和定量人血浆样品中的 PMD 对映体。

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来源期刊

Journal of chromatographic science 化学-分析化学

CiteScore

2.90

自引率

7.70%

发文量

审稿时长

5.6 months

期刊介绍： The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.