气相色谱法测定那格列奈原药中二氯甲烷和吡啶残留量

Determination of Dichloromethane and Pyridine Residues in Nateglinide by Gas Chromatography

建立气相色谱法测定那格列奈中二氯甲烷和吡啶的残留量。采用6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱,以氮气为载气,FID检测,直接进样,测定残留溶剂的含量。二氯甲烷质量浓度在0.75～36.0μg/mL范围内线性关系良好,相关系数r=0.999 9,回收率为97.45%,最低检测限为0.24μg/mL;吡啶质量浓度在0.27～12.30μg/mL范围内线性关系良好,相关系数r=0.999 6,回收率为93.49%,最低检测限为0.08μg/mL。

The gas chromatography method was obtained to determine the dichloromethane and pyridine residues in nateglinide. The residual solvent content was determined by direct injection with Cyanide by 6%-94% n-propyl-phenyl-dimethyl polysiloxane stationary phase as the capillary column, nitrogen as the carrier gas and FID as the detection device. Dichloromethane had a good linear relationship with the correlation coefficient r= 0.999 9 in the concentration of 0.75--36.0μg/mL with the recovery 97.45 % and the LOD was 0.24 μg/mL. Pyridine had a good linear rela- tionship with the correlation coefficient r= 0. 999 6 in the concentration of 0. 27--12. 30 μg/mL with the recovery of 93.49% and the LOD 0. 08μg/mL.