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  

Simultaneous Determination of 2,5-Hexanedione,Phenol and o-Cresol in Urine Samples by HPLC with Dispersive Liquid Phase Micro-extraction

作　　者：张伟亚[1] 李红丽[1] 刘丽华[1] 徐烨[1] 韩彦龙[2] 

机构地区：[1]东北大学理学院,沈阳110819 [2]承德石油高等专科学校机械工程系,承德067000

出　　处：《理化检验（化学分册）》2015年第9期1274-1277,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：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20min;③反应温度为70℃;④萃取剂三氯甲烷的用量为0.3mL;⑤萃取时间为10min。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0.3~0.7μg·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; ③temperature of reaction：70 ℃;④ amount of chloroform（extractant）：0.3mL;⑤ time of extraction：10min.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 0.3to 0.7μg·L^-1.The recovery rates measured by standard addition method were in the range of89.1%-104%,and RSD（n=7）was in the range of 3.0%-4.6%.

关 键 词：高效液相色谱法 尿样 分散液相微萃取 2 5-己二酮 苯酚 邻甲酚 

分 类 号：O652.63[理学—分析化学]