论文部分内容阅读
目的:采用顶空气相色谱法测定富马酸卢帕他定原料中的环己烷、乙酸乙酯、甲醇、二氯甲烷、三氯甲烷5种有机溶剂的残留量。方法:色谱柱:DB-WAXETRR毛细管色谱柱(30 m×0.32 mm,0.25μm);载气:氮气;FID检测器;进样口温度:200℃;采用程序升温:初始温度为35℃,保持10 min,以20℃·min~(-1)升温至220℃,保持5 min。结果:环己烷、乙酸乙酯、甲醇、二氯甲烷、三氯甲烷分别在77.590 1~698.310 9μg·ml~(-1)(r=0.999 7),102.166 6~919.499 4μg·ml~(-1)(r=0.999 8),62.744 7~564.703 2μg·ml~(-1)(r=0.999 9),12.011 2~108.101 1μg·ml~(-1)(r=0.999 6),1.262 8~11.365 6μg·ml~(-1)(r=0.999 6)范围内线性关系良好。5种残留溶剂的平均回收率分别为103.9%,103.5%,104.9%,107.1%,103.4%,RSD值分别为2.3%、2.6%、3.1%、2.8%、4.5%(n=9)。富马酸卢帕他定原料中均未检出此5种残留溶剂。结论:本方法稳定、简便、准确,灵敏度高,适用于富马酸卢帕他定原料中残留溶剂的测定。
OBJECTIVE: To determine the residues of cyclohexane, ethyl acetate, methanol, methylene chloride and trichloromethane in rupatadine fumarate by headspace gas chromatography. Method: Column: DB-WAXETRR capillary column (30 m × 0.32 mm, 0.25 μm); carrier gas: nitrogen; FID detector; inlet temperature: 200 ° C; temperature programmed: initial temperature of 35 ° C 10 min, the temperature was raised to 220 ℃ at 20 ℃ · min ~ (-1) for 5 min. Results: Cyclohexane, ethyl acetate, methanol, methylene chloride and chloroform were respectively in the range of 77.590 1 ~ 698.310 9μg · ml -1 (r = 0.999 7), 102.166 6 ~ 919.499 4μg · ml ~ (-1) (R = 0.999 8), 62.744 7 ~ 564.703 2μg · ml -1 (r = 0.999 9), 12.011 2 ~ 108.101 1μg · ml -1 (r = 0.999 6), 1.262 8 ~ 11.365 6μg · ml -1 (r = 0.999 6) within a good linear relationship. The average recoveries of the five residual solvents were 103.9%, 103.5%, 104.9%, 107.1% and 103.4%, respectively. The RSDs were 2.3%, 2.6%, 3.1%, 2.8% and 4.5%, respectively. The five residual solvents were not detected in the raw material of rupatadine fumarate. Conclusion: The method is stable, simple, accurate, sensitive and suitable for the determination of residual solvents in raw materials of rupatadine fumarate.