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.
Determination of Diethylamine and Triethylamine in Florfenicol by Gas Chromatography
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.
FlorfenicoldiethylaminetriethylamineInert Cap for Aminestest columns
NETL
NSTL
万方数据
