GC测定甲苯咪唑中的残留溶剂

Determination of Residual Organic Solvents in Mebendazole by GC

目的采用顶空气相色谱法测定甲苯咪唑原料药中的有机溶剂残留量。方法以DMF-H2O(2︰1)溶液为样品溶剂,选用Perkin Elmer气相色谱仪,配备顶空进样器和FID检测器,Agilent DB-624毛细管柱为分析柱,外标法测定。结果甲醇、乙醇、异丙醇、三氯甲烷和甲苯分别在18.7~224,46.9~562,46.9~562,1.50~17.9,2.81~33.8μg·m L-1内线性关系良好(r>0.999);各组分检出限分别为0.19,0.10,0.11,0.18,0.08μg·m L-1;各组分回收率为90.0%~110.0%。结论该方法准确、灵敏、可靠,可用于甲苯咪唑有机残留溶剂的测定。

OBJECTIVE To establish a headspace gas chromatography method for determination of residual solvents in mebendazole active pharmaceutical ingredients. METHODS The samples were dissolved in DMF-H2 O（2︰1）. Perkin Elmer gas chromatography with headspace sampling and FID detector was selected. Agilent DB-624 capillary column was used as analytical column. External standard method was used to determine the content. RESULTS A good linear correlation of methanol, alcohol, isopropanol, trichloromethane and toluenethe were shown at the range of 18.7-224, 46.9-562, 46.9-562, 1.50-17.9, 2.81-33.8 μg·mL^-1（r0.999）, respectively. Detection limit of each components were 0.19, 0.10, 0.11, 0.18, 0.08 μg·mL^-1. Recovery range were 90.0%-110.0%. CONCLUSION With good accuracy, sensitivity and reliability, the method can be used for the determination of the residual organic solvents in mebendazole.