顶空气相色谱法测定马来酸曲美布汀中溶剂残留量  

Determination of residual solvents in Trimebutine Maleate by headspace capillary GC

作　　者：吴毅彦[1] 王卫[1] 

机构地区：[1]天津市药品检验所,天津300070

出　　处：《中国药业》2013年第24期40-41,共2页China Pharmaceuticals

摘　　要：目的建立原料药马来酸曲美布汀中乙醇、异丙醇、正己烷、四氢呋喃、甲苯等6种有机溶剂的分离测定方法。方法色谱柱采用AgilentDB-624柱（30m×0．32mm，1．8汕m）；柱温为初始温度40℃，保持5min，以10℃／min速度升温至180℃，保持5min；进样口温度200℃；检测器温度250℃；载气为Nz；栽气流速为2mL／min；分流比为1：5；顶空条件为平衡温度60℃，平衡时间30rain，进样体积1mL。结果被测组分均能得到有效分离，上述溶剂在所考察的质量浓度范围内线性关系良好（r=0．9997～0．9999），回收率为99．7％～101．5％。结论该方法灵敏、准确、重复性好，可用于马来酸曲关布汀原料药中残留溶剂的测定。Objective To establish a method of headspace capillary GC for the determination of residual solvents in Trimebutine Maleate. Method The GC method was achived on a Agilent DB-624 capillary column（30 mm ~0. 32 m, 1.8 Ixm）,procedural column temperature was 40 ~C for 5 min, heated to 180 ~C at the rate of 10 ~C/min for 5 min; the inlet temperature was 200 ~C; the detector tem- perature was 250 ~C; N2 was carrier; the rate was 2 mL/min; the split ratio was 1： 5; the head space conditions were equilibrium temperature 60 ~C, eqnilibrium time 30 rain, volume 1 mL. Results The five residual solvents （ethanol, isopropanol, tetrahydrofuran, methylbenzene） were completely separated, and the linearities were fairly good（r=0.999 7-0. 999 9）.The average recoveries were 99.7%-101.5% for five residual solvents. Conclusion The method is simple, accurate and reoroducible for determination of Trimebutine Maleate.

关 键 词：马来酸曲美布汀 残留溶剂 顶空气相色谱法 

分 类 号：R927.11[医药卫生—药学] R975