气相色谱法测定2,6-二甲基苯胺中的10种相关杂质  

Separation and Determination of ten Impurities in 2,6-Dimethylaniline by Capillary Gas Chromatography

作　　者：郄一奇 韩静 汤金春 钟毓灵 张皓阅 苏梦翔 Qie Yiqi;Han Jing;Tang Jinchun;Zhong Yuling;Zhang Haoyue;Su Mengxiang(Department of Pharmaceutical Analysis,School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China;Changzhou Kangpu Pharmaceutical Co.,Ltd.,Changzhou 225600,China;Key Laboratory of Drug Quality Control and Pharmacovigilance(China Pharmaceutical University),Ministry of Education,Nanjing 210009,China;Key Laboratory for Research and Evaluation of Pharmaceutical Preparations and Excipients,National Medical Products Administration,Nanjing 210009,China)

机构地区：[1]中国药科大学药学院药物分析系,江苏南京210009 [2]常州康普药业有限公司,江苏常州225600 [3]药物质量与安全预警教育部重点实验室(中国药科大学),江苏南京210009 [4]国家药品监督管理局药物制剂及辅料研究与评价重点实验室,江苏南京210009

出　　处：《山东化工》2023年第14期119-122,126,共5页Shandong Chemical Industry

摘　　要：建立了气相色谱法同时检测2,6-二甲基苯胺中的10种相关杂质,即间二甲苯、2,4-二甲基硝基苯、2,6-二甲基硝基苯、2,3-二甲基苯胺、2,4-二甲基苯胺、2,5-二甲基苯胺、3,4-二甲基苯胺、3,5-二甲基苯胺、邻甲苯胺、对甲苯胺。色谱柱采用DB-FFAP型毛细管柱(30 m×0.25 mm×0.25μm);程序升温,起始温度为60℃,维持10 min,以15℃/min的速率升温至110℃,维持56 min,再以25℃/min的速率升温至200℃,维持10 min;进样口温度为230℃;检测器温度为235℃;流速为1.0 mL/min;分流比为10∶1。结果显示,10种杂质均分离良好;定量限分别为5μg/mL(7个杂质)、10μg/mL(2个杂质)和30μg/mL(1个杂质),且杂质在各浓度范围内线性关系良好;平均回收率(n=9)在88.17%~108.17%范围内,RSD均<10%。该方法操作简便,专属性、精密度良好,可用于2,6-二甲基苯胺中相关杂质的准确测定。In this paper,a gas chromatography method was developed,optimized and validated for the determination of ten impurities namely m-Xylene,2,4-Dimethylnitrobenzene,2,6-Dimethylnitrobenzene,2,3-Dimethylaniline,2,4-Dimethylaniline,2,5-Dimethylaniline,3,4-Dimethylaniline,3,5-Dimethylaniline,o-Toluidine and p-Toluidine in 2,6-Dimethylaniline samples.The determination was performed on a DB-FFAP(30 m×0.25 mm×0.25μm)column and good separation was obtained using a programmed temperature mode.The method was validated according to the ICH guidelines.The limits of quantification were 5,10 and 30μg/mL,respectively.All impurities showed good linearity over the concentration range of LOQ to 200μg/mL,with correlation factors([WT5"BX]r)more than 0.990.The average recoveries ranged from 88.17%to 108.17%,[WT5"BX]RSD<10%.The results of precision,robustness and solution stability were also within acceptable limits.Furthermore,the method was successfully applied to three batches of commercial samples.In conclusion,the established method is simple,accurate and can be used for the quality control of 2,6-Dimethylaniline.

关 键 词：2 6-二甲基苯胺 有关物质 异构体杂质 气相色谱法 方法学验证 

分 类 号：O657.71[理学—分析化学] TQ450.7[理学—化学]