GC法检测氟康唑原料药中的有机溶剂残留量

目的:建立检测氟康唑原料药中有机溶剂残留量的方法。方法:采用气相色谱法。色谱柱为DB-17毛细管柱,柱温采用程序升温,载气为N2,氢火焰离子化检测器,测定原料药中残留溶剂丙酮、乙酸乙酯、甲苯。结果:丙酮、乙酸乙酯、甲苯的检测浓度线性范围分别为128～2555(r=0.9997)、130～2589(r=0.9995)、27～530μg·mL-(1r=0.9991);平均回收率分别为98.1%、98.0%、97.5%,RSD分别为2.3%、1.3%、1.5%,最低检测限分别为11、7.1、0.6ng;3批样品中均未检出3种有机溶剂。结论:所建立的方法简便、灵敏、准确,能够有效分离和准确检测氟康唑原料药中的有机溶剂残留量。

Content Determination of Residual Organic Solvents in Fluconazole Crude Drugs by GC

ABSTRACT OBJECTIVE： To establish a method for the content determination of residual organic solvents in fluconazole. METHODS： GC method was adopted. The determination was performed on DB-17 capillary column using nitrogen gas as cartier gas and FID as detector. The temperature-programmed method was adopted. The contents of residual acetone, ethyl acetate, methyl- benzene in crude drugs were determined. RESULTS： The linear ranges of residual solvents acetone, ethyl acetate and methylbenzene were 128～2 555μg·mL^-1（r=0.999 7）, 130～2 589μg·mL^-1 （r=0.999 5）, 27～530μ·mL^-1 （r=0.999 1）. And their recoveries were 98.1%, 98.0% and 97.5%, respectively. RSDs were 2.3%, 1.3% and 1.5%. The minimum detection limits were 11 ng, 7.1 ng and 0.6 ng, respectively. 3 kinds of above organic solvents were not found in 3 batches of samples. CONCLUSION： This method is simple, sensitive and accurate, and suitable for content determination of residual solvents in fluconazole.