固相萃取-气相色谱-质谱法分析尿液中邻苯二甲酸单酯和双酯  

Determination of phthalate monoesters and diesters in urine by solid-phase extraction and gas chromatography-mass spectrometry

作　　者：林兴桃[1] 王小逸[1] 赵靖强[1] 

机构地区：[1]北京工业大学环境与能源工程学院,北京100124

出　　处：《色谱》2016年第5期528-532,共5页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(21177004)~~

摘　　要：建立了固相萃取-气相色谱-质谱测定尿液中邻苯二甲酸单酯和双酯的分析方法。尿液经β-葡萄糖苷酸酶酶解后进行固相萃取净化,用乙腈、乙酸乙酯和乙醚-正己烷（1∶19,v/v）分别洗脱,合并洗脱液,氮气吹干后,用N,O-双三甲基硅基三氟乙酰胺（BSTFA）对邻苯二甲酸单酯进行硅烷化处理,使用气相色谱-质谱法检测。邻苯二甲酸单酯和双酯的线性范围为5-1 000μg/L,检出限为0.3-1.1μg/L,回收率为77.9%-97.7%,相对标准偏差为3.7%-10.9%。应用该方法对50份尿液进行检测,检出邻苯二甲酸二（2-乙基己基）酯（DEHP）等7种邻苯二甲酸单酯和双酯类物质,平均质量浓度为6.0-142.7μg/L。该方法准确、可靠、灵敏度高,适用于尿液中邻苯二甲酸单酯和双酯的同时测定。A method for the determination of phthalate monoesters and diesters in urine by solid-phase extraction and gas chromatography-mass spectrometry（SPE-GC-MS） was developed. After urine enzymatic hydrolysis by β-glucuronidase,the sample was pretreated by SPE. Phthalate monoesters and diesters were eluted by acetonitrile,ethyl acetate and ethyl ester-n-hexane（1 ∶19,v/v）,separately. The mixture of the elution was dried by N2 and derivatized with N,O-bis（trimethylsilyl）trifluoroacetamide before GC-MS analysis. Good linear relationships were obtained in the range of 5-1 000 μg/L. The limits of detection were between0. 3 and 1. 1 μg/L. The recoveries of phthalate monoesters and diesters were in the range of77. 9%-97. 7% and the relative standard deviations（RSDs）were 3. 7%- 10. 9%. The method was applied to analyze 50 urine samples. Seven compounds,such as di-2-ethylhexyl phthalate（DEHP）,were detected. The mean concentrations were between 6. 0 and 142. 7 μg/L. The method is highly accurate,reliable and sensitive for monitoring phthalate monoesters and diesters in urine.

关 键 词：气相色谱-质谱 固相萃取 化学衍生 邻苯二甲酸单酯 邻苯二甲酸双酯 尿液 

分 类 号：O658[理学—分析化学]