固相萃取-高效液相色谱法测定水中邻苯二甲酸酯类的方法研究

Determination of phthalate esters in water using solid phase extraction and high performance liquid chromatography

建立了固相萃取-高效液相色谱法测定水中5种邻苯二甲酸酯类的方法。通过正交实验确定了固相萃取的最优化条件：洗脱剂组成（乙醚：甲醇）19：1，洗脱速率1．0mL／min，洗脱体积9mL，清洗剂组成（甲醇：水）1：19。液相色谱的最佳条件：检测波长224nm，流速1．0mL／min，采用梯度洗脱，开始时甲醇-水（75：26，V／V），保持6min，第7min甲醇比例上升到100％。结果，5种物质峰面积对浓度进行线性回归的相关系数均大于0．9992，该方法的最低检出限在（0．01～0．07）pg／L之间，加标回收率82．1％～97．4％，相对标准偏差（RSD）1．1％～2．4％。

A method for the determination of 5 kinds of phthalate esters in water by using solid-phase extracti -on （SPE） and high performance liquid chromatogram -phy （HPLC） was established. Several factors that would affect recoveries of analytes were optimized by orthogonal design. The optimized results of SPE were as follows： eluting solvent was V（methanol）： V（ethy-lether）=1： 19, eluting rate 1.0mL/min, elution volume 9mL, and washing solvent was V（methanol）： V（H20）= 1： 19. The optimized results of HPLC were as follows： detection wave was 224nm and rate was 1.0mL/min. Use gradient elution. At the beginning, the flow phase was V（methanol）： V（H2O）=75：25 and kept it for 6rain. The proportion of methanol rose to 100% at the 7min.Linear correlation coefficient （r） was over 0.9992.The limits of detection were between 0.01 and 0.07 ug / L. The recoveries of five phthalates acid esters were between 82.1%-97.4%. The limits of detection relative standard deviation was between 1.1%-2.4%.