气相色谱法测定非布索坦中残留有机溶剂含量  

Determination of Residual Organic Solvents in Febuxostat by GC

作　　者：王辉[1] 常先平 周成钥[3] 吕凌[1] 丁姗姗[4] 

机构地区：[1]安徽省药物研究所.安徽省缓控释工程技术研究中心,安徽合肥230022 [2]安徽省蚌埠市怀远县人民医院药剂科,安徽蚌埠233400 [3]安徽医科大学,安徽合肥230031 [4]安徽中医学院,安徽合肥230031

出　　处：《中国药业》2012年第22期57-58,共2页China Pharmaceuticals

摘　　要：目的建立非布索坦中6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SPB-5填充柱(30 m×0.53 mm,5.0μm),载气为氮气,以N-甲基吡咯烷酮为溶剂,测定了非布索坦原料药中乙醇、二氯甲烷、乙酸乙酯、四氢呋喃、吡啶、二甲基甲酰胺的残留量。结果6种有机溶剂完全分离,在所考察的质量浓度范围内线性关系良好。其中质量浓度线性范围乙醇在129.2～1 033.6μg/mL(r=0.999 7),二氯甲烷在15.2～121.6μg/mL(r=0.999 9),乙酸乙酯在125.2～1 001.6μg/mL(r=0.999 8),四氢呋喃在18.6～148.8μg/mL(r=0.999 9),吡啶的线性范围在99.6～398.4μg/mL(r=0.999 6);二甲基甲酰胺的线性范围在25～200μg/mL(r=0.999 2)。各残留溶剂的精密度试验的RSD均小于10%。结论该试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。Objective To establish a method for the determination of six residual organic solvents in febuxostat.Methods The residual organic solvents including ethanol,dichlormethane,acetidin,tetrahydrofuran,pyridine and n,n-dimethylformamide in the raw material drug febuxostat were quantitatively determined by GC with solution direct injection on the SPB-5 packed column（30 m × 0.53 mm,5.0 μm）.The carrier gas was nitrogen with methyl-2-pyrrolidinone as the solvent.Results Six residual organic solvents were completely separated.The linear ranges were 129.2-1 033.6 g / mL（r = 0.999 7） for ethanol,15.2-121.6 μg / mL（r = 0.999 9） for dichlormethane,125.2-1 001.6 μg / mL（r = 0.999 8） for acetidin,18.6-148.8 μg / mL（r = 0.999 9） for tetrahydrofuran,99.6-398.4 μg / mL（r = 0.999 6） for pyridine,25-200 μg / mL（r = 0.999 2） for n,n-dimethylformamide.RSD of precision for six residual organic solvents was less than 10%.Conclusion The established method is simple,sensitive,accurate and can be used for the determination of residual solvents in febuxostat.

关 键 词：非布索坦 气相色谱法 残留有机溶剂 

分 类 号：R927.11[医药卫生—药学] R971.1