顶空气相色谱法测定埃索美拉唑镁中的残留溶剂

Determination of Residual Solvents in Esomeprazole Megnesium by Headspace Gas Chromatography

目的建立测定埃索美拉唑镁中残留溶剂(甲醇、二氯甲烷、甲苯)的顶空气相色谱法。方法采用火焰离子化检测器,以二甲亚砜为溶剂,通过对色谱条件优化,建立了ZB-624为色谱柱、平衡温度为80℃、平衡时间为45 min的残留溶剂测定方法。结果经方法学验证,上述3种溶剂的方法检出限分别为0.304 6,0.433 7,0.094 63μg·mL^(-1);平均回收率为97.3%~109.6%;相关系数均大于0.999 0。结论该方法的检测灵敏度高、精密度好、准确度高、线性关系良好,可用于埃索美拉唑镁中残留溶剂的测定。

OBJECTIVE A headspace gas chromatographic method is established and validated for the determination of residual solvents of methanol,dichloromethane,and toluene. METHODS The samples were analyzed by using FID as the detector and dimethyl sulfoxide as sample solvent. The detection of residual solvents was performed on a ZB-624 capillary column with vial equilibration temperature of 80 ℃ and equilibration time of 45 min. RESULTS The limits of detection（ LOD） for methanol,dichloromethane,and toluene were 0.304 6,0.433 7,0.094 63 μg·mL^（-1）,respectively. The average recoveries were in the range of 97.3%-109.6%,and the correlation coefficients were above 0. 999 0. CONCLUSION The method showe the advantages of high sensitivity,good accurancy,linearity and can be used for the determination of residual solvents in esomeprazole megnesium.