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GC法同时测定6-异喹啉甲酸-5,7-二氯-1,2,3,4-四氢盐酸盐中7种残留含量

Simultaneous Determination of Seven Residues in 6-isoquinoline Formic Acid-5,7-dichloro-1,2,3,4-tetrahydro Hydrochloride by GC
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摘要 目的:建立了气相色谱法用于测定立他司特的关键起始物料6-异喹啉甲酸-5,7-二氯-1,2,3,4-四氢盐酸盐中有机溶剂无水乙醇、异丙醇、叔丁醇、甲基叔丁基醚、四氢呋喃、四甲基乙二胺、正庚烷残留量的方法。方法及结果:表明在CP7447色谱柱上七种残留溶剂能与其他组分分离良好。七种残留溶剂在配置浓度范围内,r≥0.996,呈现良好的线性关系。七种残留溶剂平均回收率(n=9)为102.5%~105.5%,RSD均≤5.5%。结论:此方法结果准确、可靠,可用于立他司特的关键起始物料6-异喹啉甲酸-5,7-二氯-1,2,3,4-四氢盐酸盐中七种残留溶剂的测定。 Objective:A gas chromatographic method was developed for the determination of the residual amounts of the organic solvents anhydrous ethanol,isopropanol,tert-butanol,methyl tert-butyl ether,tetrahydrofuran,tetramethylethylenediamine,and n-heptane in 6-isoquinolinecarboxylic acid-5,7-dichloro-1,2,3,4-tetrahydrohydrohydrochloride,a key starting material of ritazanolast.Methods and Results:It was shown that the seven residual solvents could be well separated from the other components on a CP7447 column.The seven residual solvents showed good linearity in the configured concentration range with r≥0.996.The average recoveries of the seven residual solvents(n=9)ranged from 102.5%to 105.5%with the RSD less than 5.5%.Conclusion:This method is accurate and reliable,and can be used for the determination of seven residual solvents in 6-isoquinolinecarboxylic acid-5,7-dichloro-1,2,3,4-tetrahydrohydrochloride,which is the key starting material of ritalinostat.
作者 张冰 李思琦 马长沙 Zhang Bing;Li Siqi;Ma Changsha(School of Pharmacy,Yanbian University,Jilin,136200;Jilin Bodaweiye Pharmaceutical Research Co.,Ltd.,Jilin,130000)
出处 《当代化工研究》 CAS 2024年第20期76-78,共3页 Modern Chemical Research
关键词 立他司特 6-异喹啉甲酸-5 7-二氯-1 2 3 4-四氢盐酸盐 残留溶剂 GC lifitegrast 6-Isoquinolinecarboxylic acid-5,7-dichloro-1,2,3,4-tetrahydrochloride residual solvents gas chromatography
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