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Enantioseparation of Citalopram by RP-HPLC Using Sulfobutyl Ether-β-Cyclodextrin as a Chiral Mobile Phase Additive

机译:磺丁基醚-β-环糊精作为手性流动相添加剂的RP-HPLC对映体拆分西酞普兰

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摘要

Enantiomeric separation of citalopram (CIT) was developed using a reversed phase HPLC (RP-HPLC) with sulfobutylether-β-cyclodextrin (SBE-β-CD) as a chiral mobile phase additive. The effects of the pH value of aqueous buffer, concentration of chiral additive, composition of mobile phase, and column temperature on the enantioseparation of CIT were investigated on the Hedera ODS-2 C18 column (250 mm × 4.6 mm × 5.0 um). A satisfactory resolution was achieved at 25°C using a mobile phase consisting of a mixture of aqueous buffer (pH of 2.5, 5 mM sodium dihydrogen phosphate, and 12 mM SBE-β-CD), methanol, and acetonitrile with a volumetric ratio of 21 : 3 : 1 and flow rate of 1.0 mL/min. This analytical method was evaluated by examining the precision (lower than 3.0%), linearity (regression coefficients close to 1), limit of detection (0.070 µg/mL for (R)-CIT and 0.076 µg/mL for (S)-CIT), and limit of quantitation (0.235 µg/mL for (R)-CIT and 0.254 µg/mL for (S)-CIT).
机译:西酞普兰(CIT)的对映体分离是采用反相HPLC(RP-HPLC),其中磺基丁基醚-β-环糊精(SBE-β-CD)作为手性流动相添加剂。在Hedera ODS-2 C18色谱柱(250 mm×4.6 mm×5.0 um)上研究了水性缓冲液的pH值,手性添加剂的浓度,流动相的组成和柱温对CIT对映体分离的影响。在25°C下使用流动相(由水缓冲液(pH为2.5、5 aqueousmM磷酸二氢钠和12 mMSBE-β-CD),甲醇和乙腈的混合物组成)的流动相实现了令人满意的分离度21:3:1,流速为1.0毫升/分钟。通过分析精密度(低于3.0%),线性(回归系数接近1),检出限((R)-CIT为0.070μg/ mL和(S)-CIT为0.076μg/ mL)来评估该分析方法。 )和定量限((R)-CIT为0.235μg/ mL,(S)-CIT为0.254μg/ mL)。

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