毛细管电泳法测定(S)-2-(6-羟基-2,3-二氢苯并呋喃-3-基)乙酸甲酯中R异构体

目的建立毛细管电泳法测定(S)-2-(6-羟基-2,3-二氢苯并呋喃-3-基)乙酸甲酯中R异构体的方法。方法采用毛细管电泳法。以磺酸-β-环糊精(S-β-CD)为选择剂;25 mmol/L硼酸盐缓冲液(pH 8.9,含S-β-CD 1.8%)为运行缓冲液;运行电压为25 kV;柱温为15℃;检测波长:214 nm;3.4 kPa压力进样10 s。结果 (S)-2-(6-羟基-2,3-二氢苯并呋喃-3-基)乙酸甲酯与R异构体的分离度为2.9。R异构体在2~30μg/m L与峰面积线性关系良好(r=0.999 5),平均回收率为96.6%,RSD值为4.9%(n=6)。结论建立的毛细管电泳法操作简便,结果准确可靠,可用于(S)-2-(6-羟基-2,3-二氢苯并呋喃-3-基)乙酸甲酯中R异构体的控制。

Determination of R isomer in (S)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl) acetate by capillary electrophoresis

ObjectiveTo establish a capillary electrophoresis method for the determination ofR-optical isomer in (S)-methyl- 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate.MethodsCapillary electrophoresis method was adopted. Sulfate-β-cyclodextrin (S-β-CD) was used as selector. The background buffer was 25 mmol/L borate buffer solution (pH 8.9, containing 1.8% S-β-CD). The separation was performed at 15℃ with the voltage of 25 kV and the wavelength was 214 nm. Pressure was 3.4 kPa and injected for 10 s. Results(S)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate and itsR-enantiomer were basely resolved with resolution of 2.9. The calibration curve ofR-enantiomer was linear in the concentration range of 2 — 30μg/mL (r= 0.9995). The average recovery was 96.6% with RSD 4.9% (n= 6).Conclusion The method is convenient, rapid, accurate, and can be used for the determination of (R)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate in (S)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran- 3-yl) acetate.