孕妇尿液中五种邻苯二甲酸酯代谢产物的固相萃取-高效液相串联质谱测定法  

Determination of five kinds of phthalate metabolites in urine of pregnant women by solid-phase extraction high performance liquid chromatography-tandem mass spectrometry

作　　者：蔡岩[1] 杨叶[1] 燕美玲[1] 王玮[1] 陈曦[1] 孙增荣[1] 

机构地区：[1]天津医科大学公共卫生学院,天津300070

出　　处：《环境与健康杂志》2013年第1期61-63,共3页Journal of Environment and Health

基　　金：天津市科技支撑计划重点项目(09ZCGYSF01700)

摘　　要：目的建立人体尿液中5种邻苯二甲酸酯代谢产物的固相萃取-高效液相串联质谱测定法。方法尿液中5种邻苯二甲酸酯代谢产物经β-葡萄糖苷酸酶水解后，采用NEXUS固相萃取柱富集，乙腈-乙酸乙酯（体积比1：2）洗脱，苯基柱分离，在正电离模式下利用质谱的多反应监测模式进行定性和定量分析。结果该方法在0．3-800μg／L范围内线性关系良好，标准曲线回归方程相关系数均〉0．99；孕妇尿中邻苯二甲酸单甲酯（MMP）、邻苯二甲酸单乙酯（MEP）、邻苯二甲酸单丁酯（MBP）、邻苯二甲酸单丁苄酯（MBzP）、邻苯二甲酸单（2-乙基己基）酯（MEHP）的最低检出限分别为1．16、1．00、0．53、0．14、0．22μg／L，加标回收率为95．36％-98．13％，相对标准偏差（RSO）为0．36％～3．75％。结论该方法精密度和重现性良好，回收率高，检出限较低，可用于人体尿液中多种邻苯二甲酸酯代谢产物的同时检测。Objective To establish a method for determination of five kinds of phthalate metabolites in human urine simultaneously, and on this basis to understand the exposure level of phthalates （PAEs） in pregnant women. Methods The phthalates metabolites in the urine samples were hydrolyzed by glucuronidase, and then were concentrated by offline solid- phase extraction and eluted by acetonitrile/ethyl acetate （1：2, V/V）. After chromatographic separation on phenyl column, the analytes were qualitatively and quantitatively determined by multiple reaction monitor mode. Results The linear range of the method was 0.3-800 Ixg/L, the correlation coefficients of standard curve were higher than 0.99. The limits of detection for monomethyl phthalate （MMP）, monoethyl phthalate（MEP）, mono-n-butyl phthalate （MBP）,monobenzyl phthalate （MBzP） and mono （2-ethylhexyl） phthalate （MEHP） were 1.16, 1.00, 0.53 , 0.14 and 0.22 μg/L respectively. The recovery rates ranged from 95.36% to 98.13% and the relative standard deviations were from 0.36% to 3.75%.The detectable rates of MMP, MEP, MBP, MBzP and MEHP in 30 urine samples of pregnant women were 96.67%, 100%, 76.67%, 73.33% and 100% respectively,and their medians were 45.49, 12.21, 5.35, 0.62 and 38.63 μg/L respectively. Conclusion This method has good recovery rate, reproducibility, lower detection limit and can be used for the determination of several kinds of phthalate metabolites in human urine.

关 键 词：色谱法 液相 邻苯二甲酸酯 代谢产物 固相萃取 质谱 

分 类 号：O657.7[理学—分析化学]