摘要
目的:建立了顶空气相色谱法同时测定马来酸阿法替尼中乙醇、乙酸丁酯、四氢呋喃、二氯甲烷、甲基环己烷、甲基叔丁基醚6种残留溶剂的残留量,并使用该方法测定本品7批样品中的残留溶剂。方法:用6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱为色谱柱;起始柱温设置为40℃,保持8分钟,以10℃/min的速率升至180℃,保持8分钟;检测器为FID,检测器温度设置为220℃;柱流量设置为3.0 mL/min(恒流模式);分流比设置为5∶1;顶空瓶平衡温度为80℃,定量环温度为110℃,传输线温度为130℃,平衡时间为30 min。结果:6种残留溶剂均能有效分离,乙醇、乙酸丁酯、四氢呋喃、二氯甲烷、甲基环己烷、甲基叔丁基醚在各自限度浓度的20%~150%范围内线性关系良好(r≥0.9980);回收率均在91.3%~107.4%之间;定量限在0.154~3.43μg/mL之间。本品多批次样品中均未检出乙酸丁酯、四氢呋喃、二氯甲烷、甲基环己烷、甲基叔丁基醚,乙醇的检出量在0.02%~0.06%之间,均小于限度的30%。结论:该方法操作简便、灵敏度高、专属性强、重复性好、准确度高,可以用来对马来酸阿法替尼中乙醇、乙酸丁酯、四氢呋喃、二氯甲烷、甲基环己烷、甲基叔丁基醚6种残留溶剂的残留量进行检查。
Objective:To establish a HS-GC method for simultaneous detection of six residual solvents Including ethanol,butyl acetate,tetrahydrofuran,dichloromethane,methyl cyclohexane,methyl tert butyl ether in Afatinib dimaleate,and determine 6 residual solvents in 7 batches of samples.Methods:Chromatographic Column with 6%cyanopropylbenzene and 94%dimethylsiloxane as the stationary liquid,the initial column temperature is set to 40℃,and lasting for 8 minutes,after raised to 180℃at 10℃/min,after lasting for 8 minutes.The detector temperature is 220℃,the column flow rate is 1.0 mL/min,the Split Ratio is 5:1,the equilibrium temperature of the sample bottle is 80℃and the balance time of the sample bottle is 30 min.Results:Under the selected experimental method,the resolution between the solvent peaks meets the requirements.Ethanol,butyl acetate,tetrahydrofuran,dichloromethane,methyl cyclohexane,methyl tert butyl ether have good linear relationship between the range of 20%~150%of their respective limit concentrations(r≥0.9980),and the average recovery was 91.3%~107.4%,and the quantitative limit is 0.154~3.43μg/mL.And butyl acetate,tetrahydrofuran,dichloromethane,methyl cyclohexane,methyl tert butyl ether were not detected in many batches of Afatinib dimaleate,and the detection amount of ethanol is between 0.02%and 0.06%,all of which are less than 30%of the limit.Conclusion:The method has the advantages of simple detection,strong specificity,high detection sensitivity,accurate and repeatable.It can be used for the determination of 6 residual solvents in Afatinib dimaleate at the same time.
作者
崔金凤
Cui Jinfeng(Jiangsu Jinglixin Pharmaceutical Technology Co.,Ltd.,Nanjing 210000,China)
出处
《广东化工》
CAS
2024年第4期121-124,共4页
Guangdong Chemical Industry
