高效液相色谱-电喷雾电离-质谱法分析盐酸地芬尼多的相关物质

Analysis on Related Substances of Difenidol Hydrochloride by HPLC-ESI-MS

目的用高效液相色谱-电喷雾电离-质谱(HPLC-ESI-MS)法分析盐酸地芬尼多中的相关物质。方法色谱柱为C18柱(250mm×4.6mm,5μm),流动相为0.5mol/L三乙胺(用冰醋酸调pH至4.0)-甲醇(40∶60),流速为1mL/min;ZMD Micromass电喷雾质谱仪,离子源为ESI,检出模式为正离子检测,电源电压为3.0kV,电喷雾接口干燥气(N2)流速为320L/h,离子源温度为250℃。结果得到了样品总离子流以及选择离子流相应色谱峰的ESI-MS质谱图,初步鉴定出盐酸地芬尼多中的主要相关物质1,1-二苯基-4-哌啶-1-丁烯盐酸盐。结论检测结果为研究盐酸地芬尼多中相关物质的来源和提高产品质量提供了科学依据。

Objective To analyze the related substances of difenidol hydrochloride by high performance liquid chromatography （HPLC）- electrospray ionization（ESI） -mass spectrometer（MS）. Methods The analysis of the related substances of difenidol hydrochloride was carried out. The separation was spcrformed on Kromasil Cls column with 0. 5 mol/L triethylamine （adjusted to pH 4. 0 by glacial acetic acid）- methanol（40 ： 60）. The flow rate was 1 mL/min. The chromatography condition was ZMD Micromass - MS. Ion source： ESI; the detection mode： positive; the ionization voltage： 3.0 kV; the flow rate of dry gas（N2）： 320 L/h; the ion source temperature： 2500℃. Results The total ion current and each chromatographic peak of selected ion current were obtained, and resolution of these mass spectra was elucidated. The main related substance l, 1-dipheny1-4-piperdine- 1-butylenes hydrochlorate in difenidol hydrochloride was identified. Conclusion The results of determination offer the scientific data for studying the origin of the related substances of difenidol hydrochloride and improving its quality.