介孔涂层固相微萃取-高效液相色谱法测定水样中邻苯二羧酸酯化合物

Determination of phthalates by solid-phase microextraction coupled to HPLC using fibers with mesoporous coating

以苯基官能化MCM-41介孔复合体作为固相微萃取（SPME）的吸附涂层，与高效液相色谱（HPLC）联用测定了不同水样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）和邻苯二甲酸二辛酯（DOP）的含量，对SPME的吸附和解吸时间、温度、搅拌速度进行了优化，线性范围分别为1．19×10^-4～119μg／L、1．12×10^-4～112μg／L、1．05×10^-4～105μg／L和9．80×10^-5-98 μg/L，检出限依次为0．030、0．027、0．029和0．022ng／L。使用该方法测定了多种水样中邻苯二羧酸酯类化合物。

A SPME-HPLC method is proposed for the determination of DMP, DEP, DBP and DOP using a fiber with phenyl functionalized MCM-41 coating. Extraction/desorption time, extraction temperature and stirring rate for SPME have been optimized. The linear ranges are 1.19 × 10-4 - 119 μg/L, 1.12 × 10-4 - 112 μg/L, 1.05 × 10-4 105 μg/L and 9.8 × 10^-5 -98 μg/L for DMP, DEP, DBP and DOP, respectively. Corresponding limits of detection arc 0.030, 0.027, 0.029 and 0.022 ng/L. This SPME-HPLC technique was employed for practical determination of phthalates in different water samples. The sampling procedures are simple, rapid and solvent-free. High sensitivity and good precision were obtained.