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目的建立气相色谱法测定盐酸法舒地尔中有机溶剂残留量的方法。方法采用气相色谱法,FID检测器,以毛细管色谱柱SE-54(30 m×0.53 mm,5.0μm)为分析柱。柱温为程序升温,用初始柱温55℃平衡0.5 min,以40℃/min的速度升温至70℃,平衡1 min,以40℃/min的速度升温至180℃,平衡3 min程序升温分别测定甲醇、二氯甲烷。用初始柱温50℃平衡3 min,以20℃/min的速度升温至180℃,平衡3min程序升温测定N,N-二甲基甲酰胺。载气为氮气,进样口温度200℃,检测器温度250℃。结果 3种有机溶剂完全分离,在所考察的浓度范围内具有良好线性关系,3个溶剂相关系数均大于0.999 0,甲醇、二氯甲烷、N,N-二甲基甲酰胺的检测限分别为0.065 7、1.100 0、0.016 6μg/mL,平均回收率分别为99.8%、98.4%、99.1%。结论本试验建立的方法简便灵敏,结果准确可靠,适用于盐酸法舒地尔原料药中有机溶剂残留量的检测。
Objective To establish a method for the determination of residual organic solvents in fasudil hydrochloride by gas chromatography. Methods Gas chromatography and FID detector were used to analyze the capillary column SE-54 (30 m × 0.53 mm, 5.0 μm). The column temperature was programmed temperature. The initial column temperature was equilibrated at 55 ° C for 0.5 min, the temperature was raised to 70 ° C at a rate of 40 ° C / min, equilibrated for 1 min, the temperature was raised to 180 ° C at a rate of 40 ° C / min, Determination of methanol, dichloromethane. With the initial column temperature of 50 ° C equilibrium 3 min, 20 ° C / min speed heating to 180 ° C, 3min equilibrium temperature measurement of N, N-dimethylformamide. The carrier gas is nitrogen, the inlet temperature is 200 ° C and the detector temperature is 250 ° C. Results The results showed that the three organic solvents were completely separated and had good linearity in the investigated concentration range. The correlation coefficients of three solvents were all above 0.999 0. The detection limits of methanol, methylene chloride and N, N-dimethylformamide were 0.065 7,1.100 0,0.016 6μg / mL, the average recovery was 99.8%, 98.4%, 99.1%. Conclusion The method established in this study is simple, sensitive and accurate. The method is suitable for the determination of organic solvents in fasudil hydrochloride.