气相色谱法测定氟苯尼考中二乙胺和三乙胺残留  

Determination of Diethylamine and Triethylamine in Florfenicol by Gas Chromatography

作　　者：谭跃浪 胡克斌 韦晶晶 陈蕾 张俊梅 张春侠 吴寒梅 TAN Yue-lang;HU Ke-bin;WEI Jing-jing;CHEN Lei;ZHANG JUN-mei;ZHANG Chun-xia;WU Han-mei(Apeloa Pharmaceutical Co.,Ltd.,Dongyang 322118,China;Zhejiang Apeloa Tospo Pharmaceutical Co.,Ltd.,Dongyang 322118,China)

机构地区：[1]普洛药业股份有限公司,浙江东阳322118 [2]浙江普洛得邦制药有限公司,浙江东阳322118

出　　处：《精细化工中间体》2024年第3期84-88,共5页Fine Chemical Intermediates

摘　　要：建立气相色谱法测定氟苯尼考中二乙胺和三乙胺残留的方法。采用Inert Cap for Amines毛细管胺类测试柱,经惰性处理的衬管,载气为氮气,流速3.0 mL/min,分流比为5∶1,检测器为FID。结果表明:该方法中二乙胺、三乙胺与其相邻峰完全分离;对照峰面积RSD均小于2%;二乙胺的检测限浓度为1.84μg/mL,定量限浓度为3.67μg/mL,在3.67~13.76μg/mL浓度范围内线性相关系数r为0.995 9;三乙胺的检测限浓度为0.50μg/mL,定量限浓度为1.50μg/mL,在1.50~374.63μg/mL浓度范围内线性相关系数r为0.998 6;二乙胺的回收率90.7%~103.0%,三乙胺的回收率90.8%~97.3%;小幅改变色谱条件,耐用性良好。方法操作简单、准确度高、重复性好,适用于氟苯尼考中二乙胺、三乙胺残留的测定。To establish a GC method for the determination of diethylamine and triethylamine in Florfenicol.An Inert Cap for Amines column was adapted with deactivated inlet liner.Carrier gas with nitrogen at a flow rate of 3.0 mL/min,the spilt ratio was 5∶1,the detector was FID.Diethylamine or triethylamine was completely resolved from adjacent peaks.The RSD of STD peak area were less than 2%.The detection limit(LOD)was 1.84μg/mL for diethylamine and 0.50μg/mL for triethylamine.The quantitative limit(LOQ)was 3.67μg/mL for diethylamine and 1.50μg/mL for triethylamine.The linear range were 3.67~13.76μg/mL(r=0.9959)for diethylamine,1.50~374.63μg/mL(r=0.9986)for triethylamin.The recovery rate were 90.7%~103.0%for diethylamine,and 90.8%~97.3%for triethylamine.When minor chromatograph conditions modified,a good robustness was displayed.This method has good specificity,repeatability and accuracy,which is suitable for the determination of diethylamine and triethylamine in Florfenicol.

关 键 词：氟苯尼考 二乙胺 三乙胺 Inert Cap for Amines胺类测试柱 

分 类 号：TQ460.7[化学工程—制药化工] O657.71[理学—分析化学]