固相萃取-高效液相色谱法同时测定水中三种邻苯二甲酸酯

Simultaneous Determination of Three Phthalic Acid Esters in Water by High Performance Liquid Chromatography with Solid Phase Extraction

采用C18固相萃取和高效液相色谱法研究水中邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二丁酯（DBP）的萃取条件和测定条件，讨论不同的流动相中乙腈比例、检测波长、流速条件对DMP、DEP、DBP的定性和定量的影响，并对影响固相萃取效率的洗脱剂体积进行了试验研究，且成功应用在广东省珠江广州河段河涌水的检测中。结果显示，利用1．5mL的甲醇洗脱时，DMP、DEP、DBP的萃取回收率在82％～96％之间；在乙腈比例为80％、流速为0．6mL／min、检测波长为228nm的条件下，色谱峰完全分离，峰面积与DMP、DEP、DBP的浓度呈良好的线性关系（线性相关系数〉0．9995），检出限（LOD）为0．05～0．38μg/L，样品平均加标回收率在81．7％～109％之间，相对标准偏差（RSD）为2．3％-5．9％。该方法简便、快速，具有较高的测定准确度与精密度，适合于水中DMP、DEP、DBP的测定。

The separation and determination conditions of dimethyl phthalate （DMP）, diethyl wavelength and flow velocity on the quality and quantity of DBP, DEP and DMP was discussed. The volume of the eluent which affected the solid phase extraction efficiency was experimentally investigated, and the method was successfully applied to the detection of water samples from Guangzhou section of Pearl River. The results showed that the recoveries of DMP, DEP and DBP were 82% to 96% when eluting with 1.5 mL of methanol. The chromatographic peak was completely separated at the detection wavelength of 228 nm, 80% of acetonitrile and the flow velocity of 0.6 mL/min. The peak area and concentration of DMP, DEP and DBP showed good linear relationship （linear correlation coefficient greater than 0. 999 5）. The limit of detection （LOD） was 0.05 to 0.38 txg/L. The average recovery was 81.7% to 109% and the relative standard deviation （RSD） was 2.3% to 5.9%. This method is suitable for the determination of DMP, DEP and DBP in water because of its simple operation, rapid response, high accuracy and precision.