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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 To establish a headspace gas chromatographic method for the determination of residual solvents (methanol, dichloromethane, toluene) in esomeprazole magnesium. Methods Flame ionization detector and dimethyl sulfoxide (DMSO) as solvent were used to establish a method for the determination of residual solvents by using ZB-624 as a chromatographic column with an equilibrium temperature of 80 ℃ and an equilibrium time of 45 min. Results The results showed that the detection limits of these three solvents were 0.304 6,0.433 7 and 0.094 63 μg · mL -1, respectively. The average recoveries were 97.3% -109.6%. The correlation coefficients were all greater than 0.999 0. Conclusion The method has high detection sensitivity, good precision, high accuracy and good linearity. It can be used for the determination of residual solvents in esomeprazole magnesium.