分散液相微萃取-高效液相色谱法同时测定尿样中多环芳烃四种代谢产物

Simultaneous Determination of Four Polycyclic Aromatic Hydrocarbon Metabolites in Urine by Dispersive Liquid-Liquid Microextraction-HPLC

本研究建立了同时测定尿样中多环芳烃的四种代谢产物1-羟基芘、萘、1-萘酚和2-萘酚的分散液相微萃取-高效液相色谱法。确定了最佳的色谱条件,并对萃取剂种类及用量、分散剂种类及用量、萃取时间、加盐量、样品pH和挥干时间等条件进行了优化。在最佳的实验条件下,建立了四种组分的工作曲线,线性相关系数均达到0.9999,线性范围可达103,检出限(S/N=3)为0.06～0.3ng/mL,样品加标平均回收率为95.4%～105%,相对标准偏差为2.4%～3.5%。

A dispersive liquid-liquid microextraction-HPLC method was established for the simultaneous determination of four polycyclie aromatic hydrocarbon metabolites （1-hydroxypyrene） naphthalene, 1-naphthol and 2-naphthol） in urine samples. The chromatographic conditions were optimized and the experimental conditions such as extraction solvent and volume, dispersive solvent and volume, extraction time,amount of salt, pH and temperature were optimized. Under the optimal conditions, the working curves of the four components were established, the correlation coefficients were 0. 9999, and the linear ranges of the four components were up to 103. The detection limits ranged from 0.06 to 0.3 ng/mL（S/N =3）. The average recoveries of urine samples were from 95. 4% to 105% and the relative standard deviations were between 2.4 % and 3.5%.