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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
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
关键词
杂环胺
高效液相色谱法
大气颗粒物
Heterocyclic amines, high performance liquid chromatography, atmospheric particles