HPLC手性流动相添加剂法分离测定盐酸度洛西汀左旋异构体

沈卫阳; 潘端锦; 陈蓉

HPLC手性流动相添加剂法分离测定盐酸度洛西汀左旋异构体

Enantiomeric separation of duloxetine hydrochloride by HPLC using chiral mobile phase additives

摘要

摘要: 建立检查盐酸度洛西汀中左旋异构体的HPLC手性流动相添加剂法，为本品的质量控制提供有效的分析方法。通过优化手性添加剂环糊精种类和浓度、流动相pH和甲醇比例，确定实验条件为Diamonsil C₁₈柱（150 mm×4.6 mm，5 μm），10 mg/mL磺丁基醚-β-环糊精（SBE-β-CD）溶液（磷酸调pH至2.5）-甲醇（73∶27）为流动相，流速为1.0 mL/ min，柱温40 ℃，检测波长为230 nm。在选定的色谱条件下盐酸度洛西汀对映体之间的分离度为2.3。左旋异构体在1.0~50 μg/mL范围内，峰面积与浓度线性关系良好（r=0.999 9），左旋异构体平均回收率为100.8 %（RSD=1.0 %），定量限为0.02 μg。本研究建立的方法简便、准确、专属性强，可用于盐酸度洛西汀中左旋异构体的检查。

Abstract: An HPLC chiral separation method for duloxetine hydrochloride enantiomers using sulphobutylether-β-CD(SBE-β-CD)as chiral mobile phase additive was developed to control the quality of bulk drug.Based on the optimization of the influential factors，including the kind and concentration of chiral additives，the pH of the mobile phase，the ratio of methanol，the HPLC separation was carried out on a Diamonsil C₁₈ column (150 mm×4. 6 mm，5 μm) with a mobile phase of 10 mg/mL SBE-β-CD (pH 2.5，adjusted by phosphoric acid)-methanol(73∶27)，the flow rate 1.0 mL/min，the column temperature 40 °C，and the detection wavelength at 230 nm.Under the established chromatographic conditions，duloxetine hydrochloride and its (-)-enantiomer could be separated completely.The standard curve of (-)-enantiomer is linear over the range of 1-50 μg/mL with the correlation coefficient of 0.999 9.The average recovery was 100.8 % (RSD=1.0 %).The resolution of the two enantiomers was up to 2.3 and the limit of quantitation for (-)-enantiomer was 0.02 μg.The method is simple，accurate，specific，and could be used in the quality control of duloxetine hydrochloride.

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