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柱前衍生高效液相色谱法测定一乙醇胺含量
引用本文:刘念,杨洁,刘永琼,祁雯雯.柱前衍生高效液相色谱法测定一乙醇胺含量[J].当代化工,2009,38(4):433-435.
作者姓名:刘念  杨洁  刘永琼  祁雯雯
作者单位:武汉工程大学绿色化工过程省部共建教育部重点实验室,湖北武汉,430073
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)。

关 键 词:一乙醇胺  高效液相色谱法  柱前衍生  测定

Determination of Monoethanolamine by HPLC With Pre-column Derivatization
LIU Nian,YANG Jie,LIU Yong-qiong,QI Wen-wen.Determination of Monoethanolamine by HPLC With Pre-column Derivatization[J].Contemporary Chemical Industry,2009,38(4):433-435.
Authors:LIU Nian  YANG Jie  LIU Yong-qiong  QI Wen-wen
Affiliation:(Key Laboratory for Green Chemical Process of Ministry of Education, Wuhan Institute of Technology, Hubei Wuhan 430073, China)
Abstract: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 ).
Keywords:Monoethanolamine  HPLC  Pre-column derivatization  Determination
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