反相高效液相色谱梯度洗脱法测定制剂中的硝酸异山梨酯及其降解产物

硝酸异山梨酯(ISDN)为血管扩张药物,用于治疗心绞痛。其降解产物5-硝酸异山梨酯(5-ISMN)比其它冠状血管扩张剂更有效,且毒性小。Mizuno等用HPLC法研究了ISDN及其降解产物在水溶液中的稳定性,但分离时间较长。Dimov等报道用梯度HPLC法在18min内分离了硝酸单取代异山梨酯、醋酸单取代异山梨酯和硝酸、醋酸异山梨

DETERMINATION OF ISOSORBIDE DINITRATE AND ITS DEGRADATION PRODUCTS IN PHARMACEUTICALS BY GRADIENT RP-HPLC

Isosorbide dinitrate (ISDN) and its degradation products isosorbide-5-mononitrate (5-ISMN) and isosorbide-2-mononitrate (2-ISMN), in a spray formulation were separated and determined by step gradient RP-HPLC within 8 minutes. A Shimadzu LC-4A liquid chromatograph, Nucleosil C18 5 microns 150 X 4.6 mm (ID) column, SPD 2AS spectrophotometric detector at 220 nm with variable attenuation were used, the sensitivity was kept at 0.16 AUFS in the first 4.5 min and changed to 2.56 AUFS during 4.5-12 min. Solution A (70% methanol) and solution B (5% methanol) were employed as mobile phase at a flow rate of 1.0 ml/min in gradient elution. Good results could be obtained by CR 3A data module using external standard method. The recoveries were 98.20% (ISDN), 96.92% (5-ISMN) and 95.83% (2-ISMN) and the coefficients of correlation were 0.9990 (ISDN), and 0.9994 (5-ISMN and 2-ISMN).