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机构地区:[1]浙江大学药学院药物毒理与生化药学研究所,浙江杭州310058 [2]浙江大学医学院公共卫生系,浙江杭州310058
出 处:《浙江大学学报(医学版)》2009年第3期235-241,共7页Journal of Zhejiang University(Medical Sciences)
基 金:浙江省医药卫生科学研究基金计划(2008A039)
摘 要:目的:建立一种同时检测人尿样中β-雌二醇(β-E2)、双酚A(BPA)、己烯雌酚(DES)和沙丁胺醇(SAL)含量的GC/MS分析方法。方法:采用GC/MS法,EI检测器,色谱柱为DB-5MS毛细管柱。进样前尿样分别经过cleanert PCX和cleanert PEP固相萃取,吹干后衍生化。结果:β-E2在1-300 ng.ml^-1呈线性关系,BPA在1-200 ng.ml^-1呈线性关系,DES在2-300 ng.ml^-1呈线性关系,SAL在0.01-1.2μg.ml^-1呈线性关系,最低检测限分别为0.15 ng.ml^-1、0.19 ng.ml^-1、0.23 ng.ml^-1和1.0 ng.ml^-1,回收率分别为93.4%-110.5%、84.7%-104.9%、87.0%-105.4%和81.8%-96.8%。结论:本实验室合并了β-E2、BPA、DES和SAL这两类环境污染物的检测方法,而且最低检测限与单个检测方法相当,可用于同时监控和测定β-E2、BPA、DES和SAL对人体的危害。Objective: To establish a GC/MS method for analysis of β-estradiol (β-E2), bisphenol A (BPA),diethylstilbestrol (DES) and salbutamol (SAL) in human urine. Methods: Human urine samples were extracted by cleanert PCX and cleanert PEP cartridges; and derivatized after dried completely. β-E2, BPA, DES and SAL in the extracts were measured by GC/MS method with DB-5MS capillary column and EI ion-source. Results: The calibration curves for β-E2 in samples were linear over the concentration ranges of 1-300 ng · ml ^-1 ,for BPA were 1-200 ng · ml ^-1,for DES were 2-300 ng · ml ^-1and for SAL were 0.01-1.2 ng · ml ^-1. The limits of detection were 0.15ng · ml ^-1,0.19 ng · ml ^-1,0.23 ng · ml ^-1and 1.0 ng · ml ^-1 for β-E2,BPA ,DES and SAL,respectively. The assay recoveries for β-E2,BPA ,DES and SAL ranged from 93.4%110. 5%,84.7%-104.9%,87.0%-105-4% and 81.8%-96.8%,respectively. Conclusion: The established GC/MS raethod can detect β-E2, BPA, DES and SAL in urine samples simultaneously,which can be used in routine assessment and monitoring of β-E2,BPA, DES and SAL in human body.
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