【摘要】 目的建立非布索坦中4种有机溶剂残留量的分离测定方法。方法采用溶液直接进样气相色谱法,色谱柱为PEG-20M填充柱(2 m×3 mm),载气为氮气,以二甲基亚砜为溶剂,测定了非布索坦原料药中丙酮、乙酸乙酯、乙醇与N,N-二甲基甲酰胺的残留量。结果 4种有机溶剂完全分离,在所考察的浓度范围内线性关系良好,其中丙酮的线性范围在1.056~105.6μg.mL-1(r=0.999 8),乙酸乙酯的线性范围在1.028~102.8μg.mL-1(r=0.999 98),乙醇的线性范围在0.992~99.2μg.mL-1(r=0.999 8),N,N-二甲基甲酰胺的线性范围在0.361~36.1μg.mL-1(r=0.999 8)。各残留溶剂的精密度试验RSD均小于5%,平均回收率在97.75%~102.83%之间。结论本实验所建立的方法简便、灵敏、准确,可用于非布索坦中有机溶剂残留量的测定。更多还原

【Abstract】 OBJECTIVE To estabish a method for the determination of four residual organic solvents in Febuxostat.METHODS The residual organic solvents including acetone,ethyl acetate,ethanol and N,N-DMF were quantitatively determined by GC on PEG-20 M(2 m×3 mm)column.They showed good linearity within the designed range of concentration.DMSO was solvent media,N2 was the carrier gas.RESULTS Four residual organic solvents were completely separated.The linear range of acetone was 1.056～105.6 μg·mL-1(r=0.999 8),the linear range of ethyl acetate was 1.028～102.8 μg·mL-1(r=0.999 98),the linear range of ethanol was 0.992～99.2 μg·mL-1(r=0.999 8),the linear range of N,N-DMF was 0.361～36.1 μg·mL-1(r=0.9998).The RSD of precision of four residual organic solvents were less than 5%,the average recoveries were in the range of 97.75%～102.83%.CONCLUSION The method was simple,sensitive,accurate and can be used for the quality control of Febuxostat.更多还原