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).
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)
出处
《广东化工》
CAS
2023年第12期219-221,共3页
Guangdong Chemical Industry
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
aminotoluinic acid
residual solvent
content of ethanol
content of chlorobenzene
gas chromatography(GC)
headspace injection