顶空毛细管气相色谱法测定盐酸地芬尼多原料药中有机溶剂的残留量

目的:建立顶空气相色谱法测定盐酸地芬尼多原料药中乙醇、异丙醇、四氢呋喃3种有机溶剂残留量的方法。方法:色谱柱为DB-624石英毛细管柱,柱温85℃;检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为150℃;载气为氮气,流速为5.0mL·min-1;顶空进样,平衡温度为90℃,平衡时间为30min,顶空瓶加压时间为0.2min,进样时间为1min,定量环体积1mL,定量环温度100℃,传输线温度110℃。以二甲亚砜为溶解介质。结果:乙醇、异丙醇、四氢呋喃检测浓度的线性范围分别为0.005～1.0(r=0.9999)、0.005～1.0(r=0.9999)、0.0072～0.36(r=0.9998)mg·mL-1;平均回收率为98.5%～99.6%,RSD为0.7%～1.3%;3批样品中乙醇和异丙醇的残留量均为0.02%,四氢呋喃未检出,均符合《中国药典》2010年版要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于该原料药中有机溶剂残留量的测定。

Determination of Residual Organic Solvents in Difenidol Hydrochloride by Headspace Capillary GC

OBJECTIVE：To establish headspace GC method for the content determination of 3 kinds of residual organic solvents（alcohol,isopropyl alcohol and tetrahydrofuran） in difenidol hydrochloride.METHODS：The residual organic solvents were separated on DB-624 capillary column with column temperature of 85 ℃.FID was used as detector with a temperature of 250 ℃.The inlet temperature was 150 ℃.Nitrogen was used as carrier at flow rate of 5.0 mL·min-1.The equilibrium temperature was 90 ℃ lasting for 30 min.Pressurization time of vial was 0.2 min and injection time was 1 min.The volume and temperature of dosing ring were 1 mL and 100 ℃.The temperature of transmission line was set at 110℃ and DMSO was used as solvent.RESULTS：The linear ranges of alcohol,isopropyl alcohol and tetrahydrofuran were 0.005～1.0 mg·mL^-1（r=0.999 9）,0.005～1.0 mg·mL^-1（r=0.999 9）,0.007 2～0.36 mg·mL^-1（r=0.999 8）,respectively.The average recoveries were ranged from 98.5% to 99.6% with RSD ranged during 0.7%～1.3%.The residual levels of alcohol and isopropyl alcohol in 3 batches of samples were 0.02% which was up to the standard stated in Chinese Pharmacopeia（2010 edition）.Tetrahydrofuran hadn＇t been detected.CONCLUSION：The method is simple,accurate,sensitive and reproducible,and it is suitable for the content determination of residual organic solvents in difenidol hydrochloride.