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目的建立伏立康唑中有机溶剂(甲醇、乙醇、二氯甲烷、乙酸乙酯、四氢呋喃、丙酮、乙腈、石油醚)残留量的测定方法。方法采用毛细管气相色谱法,8种有机溶剂分成两组,第一组的色谱柱为SPBTM-5毛细管柱(30m×0.53mm,1.5μm),载气为氮气,以程序升温方式使甲醇、乙醇、二氯甲烷、乙酸乙酯、四氢呋喃达到完全分离;第二组的色谱柱为SupelcowaxTM-10毛细管柱(30m×0.53mm,1.0μm),载气为氮气,以程序升温方式使丙酮、乙腈、石油醚达到完全分离。结果在两种色谱条件下,8种溶剂的线性关系、精密度、准确度、灵敏度均达到要求,在伏立康唑原料药中检出了乙醇。结论所用方法快速准确,可用于伏立康唑原料药中8种有机残留溶剂的检查。
Objective To establish a method for the determination of the residues of voriconazole in organic solvents (methanol, ethanol, dichloromethane, ethyl acetate, tetrahydrofuran, acetone, acetonitrile and petroleum ether). Methods The capillary gas chromatography and eight kinds of organic solvents were divided into two groups. The first column was SPBTM-5 capillary column (30m × 0.53mm, 1.5μm), the carrier gas was nitrogen, and the temperature was programmed to make methanol, ethanol , Dichloromethane, ethyl acetate and tetrahydrofuran to achieve complete separation. The second column was a SupelcowaxTM-10 capillary column (30m × 0.53mm, 1.0μm). The carrier gas was nitrogen. Petroleum ether to achieve complete separation. Results Under the two chromatographic conditions, the linearity, precision, accuracy and sensitivity of the eight solvents were all met. Ethanol was detected in the voriconazole drug substance. Conclusion The method is rapid and accurate and can be used for the determination of eight organic residual solvents in voriconazole.