RP-HPLC法测定羟苯磺酸钙的有关物质

目的：对试行标准中羟苯磺酸钙反相高效液相色谱法有关物质进行讨论，并利用LC—Ms对其光降解产物进行初步分析。方法：色谱条件：色谱柱：SHIMADZU VP—ODS C18（4．6mm×150mm，5μm）；流动相：0．05mol·L^-1磷酸二氢铵-乙腈（98：2）；流速：1．0mL·min^-1；进样量为10斗L；检测波长为300nm；柱温：30℃。质谱条件：负离子电离（ESI-）方式，毛细管电压：2．5kv；椎孔电压：20V；源温：105℃；脱溶剂温度：400℃；脱溶剂气流速：400L·h^-1；二级扫描时碰撞能量：20eV（降解产物），10ev和20eV（羟苯磺酸钙）。结果：此条件下，羟苯磺酸钙中已知杂质氢醌和其他各降解产物与主成分的分离度和检测灵敏度均可满足试验要求，羟苯磺酸钙和已知杂质氢醌的检测限均为5ng。采用LC—MS／MS初步推断了羟苯磺酸钙光降解产物的化学结构。结论：本方法简便、快捷，可用于羟苯磺酸钙中有关物质的检查。

Determination of Related Substances of Calcium Dobesilate by RP-HPLC

Objective： To establish a method to determine related substances in calcium dobesilate. Method： SHIMADZU VP-ODS Cls （4. 6 mm×150 mm,5 μm）was adopted with acetonitrile -0. 05 mol·L^-1 ammonium phosphate monobasic （2： 98） as mobile phase at flow rate of 1.0 mL · min^-1. The injection volume was 10 μL and the detect wavelength was set at 300 nm. The column temperature was 30 ℃. The ESI - ionization mode, Capilary ：2. 5 kV ; Cone ; 20 V, Source temperature ： 105 ℃. Desolvation temperature ：400 ℃ ; Desolvation gas flow ：400 L ·h^-1 ; Collision Energy ：20 eV （ degradation）, 10 eV and 20 eV （ calcium dobesilate）. Result： Calcium dobesilate was separated well from it degradations and known impurity hydroquinone. The detection limits for hydroquinone and calcium dobesilate were 5 ng respectively. The chemical structure of the light induced degradation was primary identified by LC-MS/MS. Condusion： This method could be used for the determination of related substances of calcium dobesilate