盐酸米诺环素中相关物质的高效液相色谱-电喷雾电离-质谱分析

HPLC-Electrospray Ionization-Mass Spectrum Analysis of Minocycline Hydrochloride and Its Related Substances

目的:采用高效液相色谱-电喷雾电离-质谱法(HPLC-ESI-MS法)对盐酸米诺环素中的相关物质进行分析。方法:色谱柱为KromasilC8柱(250mm×4.6mm,5μm),流动相为0.2mol/L醋酸铵-乙腈(80∶20),流速为1mL/min;ZMDMicromass电喷雾质谱仪,离子源为ESI,检出模式为正离子检测,电离电压为3.0kV,电喷雾接口干燥气(N2)流速为320L/h,离子源温度为150℃。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,初步鉴定出盐酸米诺环素的主要相关物质A,B,C,D。结论:检测结果为研究盐酸米诺环素中相关物质来源和提高产品质量提供了科学依据。

Objective： To study the related substances of minocycline hydrochloride. Methods： Analysis of the related substances of minocycline hydrochloride was carried out by high performance liquid chromatography（HPLC）-electrospray ionlzation（ESI）- mass spectrometer（MS）. The separation was performed on Kromasil C8 column with 0. 2 mol/L ammonium acetate - acetonitrile （80 ： 20）. The flow rate was 1 mL/min. The chromatography condition was ZMD Micromass - mass spectrometer（MS）. Ion power ： ESI ; detection mode ： positive ;ionization voltage ： 3.0 kV ;the flow rate dry gas（N2）：320 L/h;ion power temperature： 150℃. Results：The total ion current and each chromatographic peak of selected ion current were obtained, and resolution of these mass spectra was elucidated. The related substances A,B,C and D in minocycline hydrochloride were identified. Conclusion： The results of determination offer the scien- tific data for studying the origin of the related substances of minocycline hydrochloride and improving its quality.