高效液相色谱法测定大气颗粒物中的杂环胺  

Determination of Heterocyclic Amines in Atmospheric Particles by Reversed Phase High Performance Liquid Chromatography

作　　者：董雪玲[1] 刘大锰[2] 高少鹏[3] 

机构地区：[1]中国地质大学材料科学与工程学院,北京100083 [2]中国地质大学能源学院,北京100083 [3]中国科学院青藏高原研究所,北京100085

出　　处：《分析化学》2009年第10期1415-1420,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.40475049);北京市自然科学基金(No.8032012)资助项目

摘　　要：建立了大气颗粒物中杂环胺的高效液相色谱检测方法。采用ODSC18色谱柱(250mm×4.6mm,5μm),乙腈-0.01mol/L三乙胺缓冲溶液(pH4.0)为流动相,非线性梯度洗脱,流速1.0mL/min,柱温30℃,紫外检测波长263nm,并优化荧光激发和发射波长条件,实现了6种杂环胺的基线分离和4种杂环胺的高灵敏度荧光检测。本方法中荧光和紫外检测器的检出限分别为0.0018～0.0084mg/L和0.093～0.609mg/L(S/N=3),相关系数在0.9920～0.9999之间,RSD小于5.9%,平均回收率为75.3%～111.6%,回收率相对标准偏差为1.7%～2.3%,具有较高的精确度和准确度。A method was developed for the determination of heterocyclic amines（HAS） in atmospheric particles by reversed phase high performance liquid chromatography using fluorescence and ultraviolet detection.An ODS-C18 column（250 mm×4.6 mm,5 μm） with temperature 30 ℃ was used.Acetonitrile-0.01 mol/L triethylamine（pH=4.0） solution were as mobile phase at a flow rate of 1.0 mL/min with a nonlinear gradient elution program.The optimizing excitation and emission fluorescence wavelength were determined with ultraviolet detection at 263 nm.The method realized the complete base-line separation of 6 HAS and high sensitive fluorescence determination of 4 HAS.Instrument detection limits were 0.0018-0.0084 mg/L（fluorescence detection） and 0.093-0.609 mg/L（ultraviolet detection）（S/N=3）.The correlation coefficients were 0.9920-0.9999.The relative standard deviations were under 5.9% and the recoveries were 75.3%-111.6% with RSD of 1.7%-2.3%.The method is simple,rapid and accurate and can be applied for the determination of HAS in atmospheric particles.

关 键 词：杂环胺 高效液相色谱法 大气颗粒物 

分 类 号：R114[医药卫生—卫生毒理学]