盐酸多塞平顺、反式异构体的高效液相色谱法分离测定

Determination of doxepin hydrochloride isomers by HPLC

目的测定盐酸多塞平原料和片剂中顺、反式异构体的含量。方法采用梯度洗脱高效液相色谱法。结果盐酸多塞平Z式异构体在22~110μg·mL^(-1),E式异构体在90~470μg·mL^(-1)范围内呈良好的线性关系,Z式异构体的平均加样回收率为99.98%,RSD=0.25%,E式异构体的平均加样回收率为100.07%,RSD=0.08%。结论方法简单准确,所选色谱条件温和,可用于盐酸多塞平异构体的分离测定。

OBJECTIVE To determine and separate the Z-and E-isomer of doxepin hydrochloride in doxepin hydrochloride materials and tablets.METHOD A gradient HPLC was adopted.The column was Shimpack C18(150×6mm,5μm),The mobile phase consisted of A(0.2mol.L^(-1) Potassium dihydrogen phosphate-methanol(65:35)) and B(0.02 mol.L^(-1) Potassium dihydrogen phosphate-methanol(40:60)),with the gradient condition was 0→30min,A 100%→25%.The flow rate was 1mL.min^(-1).The detection wavelength were 295 nm.RESULTS The calibration linear was in the range of 22~110μg·mL^(-1) for Z-isomer and 90~470μg·mL^(-1) for E-isomer,and the average recoveries were 99.98%(RSD=0.25%) for Z-isomer and 100.07%(RSD=0.08) for E-isomer respectively.CONCLUSION The method developing at a mild condition appeared to be simple,accurate for the determination and separation of Z-,E-isomer of doxepin hydrochloride.