氨甲苯酸残留溶剂检测方法研究  

Study on the Detection Method of Residual Solvents in Aminotoluinic Acid

作　　者：徐晓霞 李晓云 熊芳 李祖敏 伍忆 Xu Xiaoxia;Li Xiaoyun;Xiong Fang;Li Zumin;Wu Yi(Hunan Dongting Pharmaceutical Co.,Ltd.,Changde 415001,China)

机构地区：[1]湖南洞庭药业股份有限公司,湖南常德415001

出　　处：《广东化工》2023年第12期219-221,共3页Guangdong Chemical Industry

摘　　要：目的:建立气相色谱法同时测定氨甲苯酸原料药中乙醇、氯苯残留溶剂的方法。方法:采用6%氰丙苯基-94%二甲基硅氧烷毛细管柱(DB-624),氢火焰离子化(FID)检测器,恒温,N,N-二甲基甲酰胺为溶剂。结果:乙醇、氯苯2种溶剂在各自浓度范围保持良好的线性关系(r乙醇=0.999、r氯苯=0.998,n=6);定量限浓度分别为1μg/mL、5μg/mL;检测限浓度分别为0.5μg/mL、2.1μg/mL;平均加样回收率分别为99.8%、108.8%。结论:该方法操作简便,专属性好,结果准确可靠,重现性好,灵敏度高,可用于氨甲苯酸原料药中残留溶剂分析检测。Objective:To establish a gas chromatography method for the simultaneous determination of residual solvents such as ethanol and chlorobenzene in aminotoluinic acid(API).Method:Using a capillary column(DB-624)containing 6%cyanopropyl-94%dimethyl polysiloxane.Using a hydrogen flame ionization detector(FID),constant temperature,N,N-Dimethylformamide as solent.Results:Ethanol and chlorobenzene maintained a good linear relationship within their respective concentration ranges(r ethanol=0.999,r chlorobenzene=0.998,n=6);The limit of quantitation concentration was 1μg/mL,5μg/mL;The limit of detection concentration was 0.5μg/mL,2.1μg/mL;The average recovery rate of sample addition was 99.8%,108.8%.Conclusion:The method is simple to operate,has good specificity,accurate and reliable results,good reproducibility,and high sensitivity,and can be used for the analysis and detection of residual solvents in Aminotoluinic Acid(API).

关 键 词：氨甲苯酸 残留溶剂 乙醇含量 氯苯含量 气相色谱法 顶空进样 

分 类 号：TQ[化学工程]