摘要
建立柱前衍生高效液相色谱(HPLC)内标法测定一乙醇胺含量的方法。以C18(5μm,250mm×4.6mm)为色谱柱,V(甲醇)/V(磷酸氢二钾缓冲液)=40/60,为流动相,在流速为1.0mL/min,柱温30℃,紫外检测波长为310nm,进样量为20μL的情况下,选用衍生试剂2,4-二硝基氟苯(DNFB)将一乙醇胺样品在75℃水浴中衍生90min后进样分析。一乙醇胺在5～25μg/mL范围内质量浓度与峰面积呈良好的线性关系(r=0.9999),平均回收率102.27%,相对标准偏差为1.18%(n=5)。
An internal standard method for the separation and quantitative determination of monoethanolamine by HPLC with pre-column derivatization was presented. The determination was performed in Dionex high-performance liquid chromatograph and C18 chromatographic column （5 μm,250 mm × 4.6 mm）. The flow rate was 1.0 mL/min,the column temperature was 30 ℃ and injection was 20 μ L. The method based on pre-column derivatization with 2,4-dinitrofluorobenzene （DNFB）. The reaction was carried out at 75 ℃ for 90 min,then the derivatives were separated on reversed-phase column by elution using methanol /dipotassium hydrogen phqsphate buffer （40/60, v/v）and detected by ultraviolet measurement at wavelengths of 310 nm. The results show there is good linear relation ship between the mass concentration and the peak area of monoethanolamine in the range of 5 -25 μg/mL（r=0.9999）. The average recovery is 102.27% with the relative standard deviation of 1.18%（n=5 ）.
出处
《当代化工》
CAS
2009年第4期433-435,共3页
Contemporary Chemical Industry
关键词
一乙醇胺
高效液相色谱法
柱前衍生
测定
Monoethanolamine
HPLC
Pre-column derivatization
Determination
