【摘要】 基于吡啶与三氯乙酸的界面反应,建立了一种高效液相色谱测定尿液中三氯乙酸的分析方法。通过正交实验及方差分析确定了界面反应中各条件无明显的相关性,考察了尿样体积、衍生试剂体积、碱浓度、反应时间及温度等参数对反应的影响,并优化了色谱分离条件。在最佳实验条件下,建立了待测组分的工作曲线,测得三氯乙酸的线性范围为0.002 0~20.0 mg/L(r=0.999 7),方法检出限(S/N=3)为0.1μg/L,样品的加标回收率为91.9%~105%,相对标准偏差(RSD)为3.5%~4.6%。研究结果表明,利用这种界面反应可同时达到富集痕量待测组分及纯化样品的作用,有效地降低了方法的检出限,方法具有简便、快速、准确和对环境友好的特点。更多还原

【Abstract】 An HPLC method was developed for the determination of trichloroacetic acid in urine based on the interface reaction between trichloroacetic acid and pyridine. An orthogonal experiment was carried out and the result showed that there was no significant correlation among the factors. The derivatization conditions such as the volume of urine and reagent,alkali concentration,reaction time and temperature,and the chromatographic conditions were optimized. Under the optimal conditions, the working curves of the analyte was established,the linear range of trichloroacetic acid was between 0. 002 0 mg / L and 20. 0 mg / L,with correlation coefficient( r) of 0. 999 7 and detection limit( S / N = 3) of 0. 1 μg / L. The average recoveries of trichloroacetic acid in urine samples were in the range of 91. 9%- 105% with relative standard deviations of 3. 5%- 4. 6%. The results showed that the urine sample was simultaneously enriched and purified by using the interface reaction,and the detection limit was greatly reduced. The established method was turned out to be simple,rapid,sensitive, accurate and environment-friendly.更多还原