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目的:采用气相顶空色谱法测定马来酸氟吡汀原料药中的甲醇、乙醇和异丙醇3种有机溶剂的残留量。方法:采用DB-624(30 m×0.53 mm,3.0μm)毛细管色谱柱,载气为氮气,程序升温。FID检测器,温度为250℃。进样口温度为200℃。按外标法测定溶剂残留量。结果:甲醇,乙醇和异丙醇分别在2.182~152.74(r=0.999 1),3.546~248.22(r=0.999 8)和4.082~285.74μg·ml-1(r=0.999 7)范围内,线性关系良好;平均回收率分别为97.7%(RSD=1.5%),99.0%(RSD=1.1%),98.8%(RSD=1.1%)(n=5)。结论:本方法简便、准确,灵敏度高,适用于马来酸氟吡汀原料药中有机溶剂残留量的检测。
OBJECTIVE: To determine the residual amount of methanol, ethanol and isopropanol in three organic solvents of flupirtine maleate by GC-MS. Methods: DB-624 (30 m × 0.53 mm, 3.0 μm) capillary column was used. The carrier gas was nitrogen and the temperature was programmed. FID detector at a temperature of 250 ° C. Inlet temperature is 200 ° C. Solvent residue was determined by external standard method. Results: The linear relationship between methanol, ethanol and isopropanol ranged from 2.182 to 152.74 (r = 0.999 1), 3.546 to 248.22 (r = 0.999 8) and 4.082 to 285.74 μg · ml -1 (r = 0.999 7) The average recoveries were 97.7% (RSD = 1.5%), 99.0% (RSD = 1.1%) and 98.8% (RSD = 1.1%) (n = 5), respectively. Conclusion: The method is simple, accurate and sensitive. It is suitable for the determination of organic solvents residues in flupirtine maleate.