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采用带圆二色检测的高效液相色谱法测定肾上腺素的对映体纯度。

Determination of the enantiomeric purity of epinephrine by HPLC with circular dichroism detection.

作者信息

Kirkpatrick Douglas, Yang Jingyue, Trehy Michael

机构信息

United States Food and Drug Administration, CDER, Division of Pharmaceutical Analysis, St Louis, Missouri, USA.

出版信息

J Liq Chromatogr Relat Technol. 2017;2017:1-8. doi: 10.1080/10826076.2017.1333962. Epub 2017 May 31.

Abstract

Several hundred drug substances approved by the U.S. Food and Drug Administration are chiral molecules. For the enantiomeric purity assessment, current practice is to develop separation techniques using chiral columns or mobile phase modifiers to separate enantiomers before detection. An alternative approach is to use currently accepted HPLC assay methods and use chiral-specific detectors to confirm whether the correct enantiomer is present. In this paper, adding a circular dichroism (CD) detector to an achiral HPLC method from the US Pharmacopeia (USP) is shown to be amenable for the determination of the enantiomeric purity of epinephrine, a substance used to treat anaphylaxis. This HPLC-UV-CD approach was able to detect the inactive D-(+) enantiomer at 1% of the total epinephrine composition. The linearity, accuracy, and precision of HPLC-UV-CD were evaluated and compared to analyses using a chiral HPLC method. Additionally, an epinephrine drug product was analyzed for assay (concentration) and enantiomeric purity. The results from achiral and chiral methods were identical within the experimental error. Overall, achiral chromatography performed using a USP method with CD detection may serve as a general means of determining chiral drug enantiomer purity and avoids the need for the development of additional chiral-specific methods for each individual drug.

摘要

美国食品药品监督管理局批准的数百种药物都是手性分子。对于对映体纯度评估,目前的做法是开发分离技术,使用手性柱或流动相改性剂在检测前分离对映体。另一种方法是使用目前公认的高效液相色谱(HPLC)分析方法,并使用手性特异性检测器来确认是否存在正确的对映体。本文表明,在美国药典(USP)的非手性HPLC方法中添加圆二色性(CD)检测器,适用于测定用于治疗过敏反应的肾上腺素的对映体纯度。这种HPLC-紫外-CD方法能够检测到占总肾上腺素成分1%的无活性D-(+)对映体。对HPLC-紫外-CD的线性、准确性和精密度进行了评估,并与使用手性HPLC方法的分析进行了比较。此外,还对一种肾上腺素药品进行了含量(浓度)和对映体纯度分析。在实验误差范围内,非手性方法和手性方法的结果是相同的。总体而言,使用USP方法并结合CD检测进行的非手性色谱分析可作为测定手性药物对映体纯度的通用方法,并且无需为每种单独的药物开发额外的手性特异性方法。

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