气相色谱法测定非布索坦中残留有机溶剂的含量

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。

Determination of residual organic solvents in Febuxostat by GC

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 ug . mL-1 （ r =0. 999 8） ,the linear range of ethyl acetate was 1. 028 - 102. 8 ug. mL-1 （ r =0. 999 98） ,the linear range of ethanol was 0. 992 -99. 2 ug .mL-1 （ r =0. 999 8） , the linear range of N,N - DMF was 0. 361 - 36. 1 ug . 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.