目的建立5-甲氧色胺中4种有机溶剂残留量的分离测定方法。方法采用毛细管气相色谱法,程序升温,色谱柱为DB-35MS毛细管柱,FID检测器,N,N-二甲基甲酰胺为溶剂,同时检测了5-甲氧色胺原料药中乙酸乙酯、四氢呋喃、二氯甲烷、甲苯的残留量。结果各组分线性响应良好,r≥0.999,检测限分别为0.9、0.5、4.0、0.5ng,精密度RSD均小于2%,平均回收率为95.0%-105.0%。结论方法简便灵敏,结果准确可靠,适用于5-甲氧色胺中有机溶剂残留量的检测。
Aim To establish an assay method for the determination of four residual solvents in 5-me- thoxytrytamine by programmed-temperature capillary GC. Methods The residual solvents which are ethyl acetate, tetrahydrofuran, dichloromethane and toluene were quantitatively determined by capillary GC on DB-35MS column with N,N-dimethylformamide(DMF) as solvent media and FID as the detector. Four residual solvents were completely separated. Results There was a good linearity(r≥0.999). The detected limits in the sample were 0.5-4.0ng; the RSD of precision was less than 2% ; the average recovery rate was within the range of 95.0% 105.0%. Conclusion The method is simple, sensitive and accurate and can be used for quality control of 5-me- thoxytrytamine.