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首页> 外文期刊>Chirality: The pharmacological, biological, and chemical consequences of molecular asymmetry >Sensitivity improvement of circular dichroism detection in HPLC by using a low-pass electronic noise filter: Application to the enantiomeric determination purity of a basic drug
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Sensitivity improvement of circular dichroism detection in HPLC by using a low-pass electronic noise filter: Application to the enantiomeric determination purity of a basic drug

机译：使用低通电子噪声滤波器改善HPLC中圆二色性检测的灵敏度：在基本药物的对映体测定纯度中的应用

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摘要

The quality control of chiral drugs requires the determination of their enantiomeric purity. Nowadays, circular dichroism (CD) spectroscopy is gaining increasing importance in pharmaceutical analysis because of the commercially available CD detector in liquid chromatography. The separation of the two enantiomers of a basic drug (efaroxan) was achieved by high performance liquid chromatography using an amylose-derivated column with both UV and CD detections. A baseline-resolved separation (resolution: 5) was obtained after optimization of the mobile phase composition with hexane-ethanol-diethylamine (90:10:0.05; v/v/v). The use of a commercial low-pass electronic noise filter of the CD signal has improved the signal-to-noise ratio by a factor twelve and allowed the quantitation of each enantiomer in the 1.25-300 mu g ml(-1) concentration range. The CD linear calibration curve, expressed in terms of stereoisomer height ratio versus concentration ratio, was plotted over the 0.4-6% range. A correlation coefficient greater than 0.999 was obtained by least-squares regression and the limit of detection for the distomer/eutomer ratio was estimated at 0.14%. Although the method validation showed good repeatability on the retention times (RSD < 0.9%), on the peak height ratios (RSD < 8.7%) of each enantiomer only up to 99.2% enantiomeric purity was achieved.
机译：手性药物的质量控制要求确定其对映体纯度。如今，由于液相色谱中的商用CD检测器，圆二色性（CD）光谱在药物分析中正变得越来越重要。碱性药物（依法氧烷）的两种对映体的分离是通过高效液相色谱法，使用直链淀粉衍生的色谱柱同时检测UV和CD来实现的。使用己烷-乙醇-二乙胺（90：10：0.05; v / v / v）优化流动相组成后，获得了基线分离的分离度（分辨率：5）。 CD信号的商用低通电子噪声滤波器的使用将信噪比提高了十二倍，并允许在1.25-300μg ml（-1）浓度范围内对每种对映异构体进行定量。 CD线性校准曲线以立体异构体高度比对浓度比表示，在0.4-6％的范围内绘制。通过最小二乘回归获得大于0.999的相关系数，并且对异构体/共聚体比率的检出限估计为0.14％。尽管方法验证显示出保留时间（RSD <0.9％）的良好重复性，但每种对映体的峰高比（RSD <8.7％）只能达到99.2％的对映体纯度。

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