顶空气相色谱法测定奥利司他中残留溶剂

目的建立奥利司他原料药中有机溶剂残留量的测定方法。方法采用顶空进样毛细管气相色谱法,HP-IN-NOWAX毛细管柱（30 mm×0.32 mm,0.25μm）,以氮气为载气,用FID检测器,测定奥利司他原料药中正己烷、正庚烷、甲醇和乙腈的残留量。结果 4种有机溶剂完全分离,浓度在考察范围内与峰面积具有良好的线性关系,r为0.999 0~0.999 3,平均回收率为97.1%~101.9%,精密度RSD均小于10%,最低检出限为0.009~1.833μg/ml。结论本法快速、灵敏、准确,可用于本品中4种有机溶剂残留量的测定。

Determination of residual organic solvents in orlistat by headspace gas chromatography

Objective To establish a method for determination of four residual organic solvents in orlistat.Methods The residual organic solvents in orlistat are hexane、heptane、methanol and acetonitril.They were quantitatively determined by headspace gas chromatography（GC） on HP-INNOWAX column with FID detector,nitrogen as the carries.Results Four residual solvents were completely separated.There was a good linearity in the experimental concentration（r=0.999 0～0.999 3）.The RSD of precision was less than 10%.The average recovery rate ranged from 97.1% to 101.9%.The detection limits was between 0.009～1.833 μg/ml.Conclusion The method proves to be rapid,sensitive and accurate.It can be used for quality control for the determination of four residual organic solvents in orlistat.