固相萃取-高效液相色谱法测定儿童尿液中的邻苯二甲酸酯代谢物

Detemination of Urinary Phthalate Metabolites in Children by Solid Phase Extraction-High Performance Liquid Chromatography

建立了儿童尿液中3种邻苯二甲酸单酯的固相萃取-高效液相色谱测定法。固相萃取运用Waters OASIS HLB固相萃取柱,高效液相色谱测定时采用GP-Phenyl 120°型色谱柱,流动相为乙腈（0.2%的乙酸）∶水（0.2%的乙酸）=45∶55。测定的3种邻苯二甲酸酯代谢物分别为：邻苯二甲酸单丁酯（MBP）、邻苯二甲酸单苄基酯（MBzP）、邻苯二甲酸（2-乙基己基）单酯（MEHP）,在20～10 000μg/L的线性范围内,所得的这3种邻苯二甲酸单酯的回归方程均呈良好的线性关系,相关系数R≥0.99,检出限分别为：MBP 9.50μg/L,MBzP 10.50μg/L,MEHP 12.50μg/L。样品加标平均回收率在80.3%～90.15%之间,RSD为1.2%～3.62%。结果表明该方法回收率较高、重现性好、检出限低,适用于儿童尿液中3种邻苯二甲酸单酯的测定。

The method of high performance liquid chromatography after the pre-treatment with optimized SPE（SPE-HPLC） for the determination of 3 urinary phthalate metabolites in children was established. Phthalate metabolites were extracted from urine samples with Waters OASIS HLB SPE column, and performed chromatograph with a GP-Phenyl column（4. 6 min× 250 ram, 5 μm）, the mobile phase was acetonitrile（0. 2% acetic acid）： water（0. 2 % acetic acid） = 45： 55 （V： V）. The phthalate metabolites （MBP, MBzP and MEHP）were quantified with external standard method,over the range of 20--10 000μg/L. The correlation coefficients were ≥0. 99. The detection limits of MBP MBzP MEHP were 9.50,10. 50,12.50 μg/L,respectively. The average standard recovery rates were 80. 3% -90. 15% and the relative standard deviations were 1.2%～3.62%. This method was significant for monitoring urinary phthalate metabolites among children accurately and efficiently. It would be a useful tool for the detection of MBP, MBzP and MEHP in urine.