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采用羧甲基-β-环糊精,通过毛细管电泳法测定苯磺酸左旋氨氯地平原料药的对映体杂质。

Determination of enantiomeric impurity of levamlodipine besylate bulk drug by capillary electrophoresis using carboxymethyl-β-cyclodextrin.

作者信息

Qi Yuedong, Zhang Xiaojian

机构信息

The First Affiliated Hospital of Zhengzhou University, Zhengzhou, China,

出版信息

Cell Biochem Biophys. 2014 Dec;70(3):1633-7. doi: 10.1007/s12013-014-0106-2.

Abstract

A rapid capillary electrophoresis method using carboxymethyl-β-cyclodextrin (CM-β-CD) as chiral selector was developed and validated for the enantiomeric purity determination of levamlodipine besylate bulk drug. Several parameters for were optimized for a satisfactory enantioresolution, including pH of background electrolyte, the concentration of chiral selector, buffer concentration, capillary temperature and voltage. The highest resolution (Rs = 9.8) was obtained with 4 mM CM-β-CD dissolved in 40 mM phosphate buffer (pH 3.5), at temperature 25 °C and voltage 30 kV, normal polarity. This method was fully validated for the enantiomeric purity determination of the R-amlodipine at the 0.2 % level. The established method was validated in terms of selectivity, LOD and LOQ (0.001 and 0.003 mg mL(-1)), linearity (y = 2.8943x + 0.1386, r (2) = 0.9991), precision and accuracy (95-104 %). Finally, the method was further applied to investigate the enantiomeric purity of levamlodipine in bulk samples.

摘要

建立了一种以羧甲基-β-环糊精(CM-β-CD)为手性选择剂的快速毛细管电泳方法,并对其进行了验证,用于测定苯磺酸左旋氨氯地平原料药的对映体纯度。对几个参数进行了优化以获得满意的对映体分离度,包括背景电解质的pH值、手性选择剂的浓度、缓冲液浓度、毛细管温度和电压。在25℃、30 kV电压、正极性条件下,将4 mM CM-β-CD溶解于40 mM磷酸盐缓冲液(pH 3.5)中,获得了最高分辨率(Rs = 9.8)。该方法在0.2%水平下对R-氨氯地平的对映体纯度测定进行了全面验证。所建立的方法在选择性、检测限和定量限(0.001和0.003 mg mL(-1))、线性(y = 2.8943x + 0.1386,r(2) = 0.9991)、精密度和准确度(95-104%)方面均得到了验证。最后,该方法进一步应用于研究原料药中左旋氨氯地平的对映体纯度。

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