摘要
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.
出处
《上海交通大学学报(农业科学版)》
2014年第4期82-87,共6页
Journal of Shanghai Jiaotong University(Agricultural Science)
基金
上海市科学技术委员会项目(11DZ2210800)
上海儿童医学中心-雅培/世界健康基金会临床营养发展中心(AFINS)项目(AFINS-HOPE-2012-03)
上海张江国家自主创新示范区专项发展资金重点项目(201209-SJ-A0-001)