摘要
目的:建立盐酸法舒地尔原料中异构体杂质的含量测定方法。方法:采用HPLC法,色谱柱:以苯基键合硅胶为填充剂的Kromasil 100-5 Phenyl C_(18)柱(250 mm×4.6 mm,5μm),流动相:磷酸缓冲盐(10 mmol·L-1磷酸二氢铵,用1%磷酸调p H至4.0)-乙腈(80∶20),检测波长:275 nm,柱温:40℃,流速:1.0 ml·min^(-1),进样量:10μl。结果:盐酸法舒地尔及其异构体杂质分别在0.151~3.018μg·ml^(-1)(r=1.000 0)和0.101~2.014μg·ml^(-1)(r=1.0000)浓度范围内线性关系良好;盐酸法舒地尔异构体杂质的平均回收率为101.9%,RSD为0.98%(n=9)。结论:该法简便、准确好、灵敏度强,可作为盐酸法舒地尔原料异构体杂质的质量控制方法。
Objective： To establish an HPLC method for the determination of isomeric impurity in fasudil hydrochloride. Methods：The chromatographic method was carried out on a Kromasil 100-5 Phenyl C_（18） column with phenyl bonded silica as the filler（ 250 mm×4.6 mm,5 μm）,and phosphate buffer（ 10 mmol·L^（-1）ammonium dihydrogen phosphate,adjusting p H to 4.0 with 1% phosphoric acid）- acetonitrile（ 80 ∶ 20） was used as the mobile phase. The detection wavelength was 275 nm and the column temperature was40℃. The flow rate was 1.0 ml·min^（-1）,and the injection volume was 10 μl. Results： Fasudil hydrochloride and its derivative was linear within the range of 0.148-2.960 μg·ml^（-1）（ r= 1.0000） and 0.101-2.014μg·ml^（-1）（ r= 0.999 9）,respectively. The average recovery of isomer impurity in fasudil hydrochloride was 101.9% with RSD of 0.98%（ n = 9）. Conclusion： The method is simple,accurate and reproducible,which can be used for the quality control of fasudil hydrochloride and its isomer.
出处
《中国药师》
CAS
2016年第4期819-821,共3页
China Pharmacist
