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
谭跃浪 1胡克斌 1韦晶晶 2陈蕾 2张俊梅 2张春侠 1吴寒梅1
作者信息
- 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
- 折叠
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1.84 μg/mL,定量限浓度为3.67 μg/mL,在3.67～13.76 μg/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0.50 μg/mL,定量限浓度为1.50 μg/mL,在1.50～374.63 μg/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.
Abstract
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 1.84 μg/mL for diethylamine and 0.50 μg/mL for triethylamine.The quantitative limit(LOQ)was 3.67 μg/mL for diethylamine and 1.50 μg/mL for triethylamine.The linear range were 3.67～13.76 μg/mL(r=0.995 9)for diethylamine,1.50～374.63 μg/mL(r=0.998 6)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Key words
Florfenicol/diethylamine/triethylamine/Inert Cap for Amines/test columns引用本文复制引用
出版年
2024
NETL
NSTL
万方数据