提出了分散液相微萃取-高效液相色谱法同时测定尿样中2,5-己二酮、苯酚及邻甲酚的含量。优化的试验条件如下:① 衍生试剂为2,4-二硝基苯肼;② 反应时间为20 min;③ 反应温度为70 ℃;④ 萃取剂三氯甲烷的用量为0.3 mL;⑤ 萃取时间为10 min。以C18色谱柱为固定相,用不同比例的甲醇-水溶液为流动相进行梯度洗脱,用紫外检测器测定。2,5-己二酮、苯酚及邻甲酚在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.3~0.7 μg·L-1之间。加标回收率在89.1%~104%之间,测定值的相对标准偏差(n=7)在3.0%~4.6%之间。

A method of HPLC with dispersive liquid phase micro-extraction was proposed for the simultaneous determination of 2,5-hexanedione, phenol and o-cresol in urine samples. The optimized conditions found were as follows: ① derivative reagent: 2,4-dinitrophenylhydrazine; ② time of reaction: 20 min; ③ temperature of reaction: 70 ℃; ④ amount of chloroform (extractant): 0.3 mL; ⑤ time of extraction: 10 min. A C18 chromatographic column was used as stationary phase with mixtures of methanol and water with different mixing ratios as mobile phase in the gradient elution. A UV detector was used. Linear relationship between the peak area and the mass concentration of 2,5-hexanedione, phenol and o-cresol kept in definite ranges. Detection limits (3S/N) ranged from 0.3 to 0.7 μg·L-1. The recovery rates measured by standard addition method were in the range of 89.1%-104%, and RSD (n=7) was in the range of 3.0%-4.6%.