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目的:建立CE法检查手性药物佐米曲普坦中的对映异构体杂质[(R)-佐米曲普坦]。方法:在20 mmol/L磷酸二氢钠缓冲液中加入1%磺化β-环糊精,溶解后,用磷酸调节pH至3.50,作为运行缓冲液;石英毛细管60 cm(有效长度51.5 cm)×50μm ID;分离柱温为20℃;操作电压为-30 kV;气压进样(50 mbar,6 s);检测波长为220 nm。结果:佐米曲普坦与其对映异构体的分离度为6.66,(R)-佐米曲普坦浓度在4~80μg/mL范围内线性良好(相关系数为0.999 8),进样精密度为2.83%,平均加样回收率为99.97%(n=9),检测限为1.5μg/mL,磺化β-环糊精与(R)-佐米曲普坦、佐米曲普坦形成包容络合物的结合常数分别为964和905 mol-1。结论:该方法可用于佐米曲普坦的对映异构体杂质检查与结合常数的测定。
OBJECTIVE: To establish a CE method for the enantiomeric impurity detection of zolmitriptan in chiral drugs [(R) -Zolmitriptan]. Methods: 1% sulphonated β-cyclodextrin was added to 20 mmol / L sodium dihydrogen phosphate buffer and dissolved with phosphoric acid to adjust the pH to 3.50 for running buffer. The quartz capillary 60 cm (effective length 51.5 cm) × 50μm ID; the column temperature was 20 ℃; the operating voltage was -30 kV; the pressure was injected at 50 mbar for 6 s; the detection wavelength was 220 nm. Results: The separation of zolmitriptan and its enantiomer was 6.66. The concentration of (R) -Zolmitriptan was linear in the range of 4-80 μg / mL (correlation coefficient: 0.999 8). The injection precision The average recovery was 99.97% (n = 9), the detection limit was 1.5μg / mL. The sulfonated β-cyclodextrin and (R) -Zolmitriptan, The binding constants for the formation of inclusion complexes were 964 and 905 mol-1, respectively. Conclusion: This method can be applied to the determination of enantiomer impurity and determination of the binding constant of zolmitriptan.