Tang Zigang, Chu Lanling, Wang Yu, Song Yuan, Liu Ping, Fan Jinhui, Huang Jinjin, Liu Xiongwei, Wei Lanlan, Li Chen, Zhao Renshan, Kang Xuejun
Key Laboratory of Environmental Medicine and Engineering (Ministry of Education), School of Public Health, Southeast University, Nanjing 210096,China.
Key Laboratory of Child Development and Learning Science (Ministry of Education), School of Biological Science and Medical Engineering, Southeast University, Nanjing 210096, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 1;1061-1062:342-348. doi: 10.1016/j.jchromb.2017.07.030. Epub 2017 Jul 18.
In this paper, we developed a rapid and safe method based on packed-fiber solid-phase extraction (PFSPE) system coupled with gas chromatography-mass spectrometry for the determination of four phthalate esters (PAEs), diethyl-o-phthalate (DEP), dibutyl-o-phthalate (DBP), di (2-ethylhexyl) phathalate (DEHP), di-n-octyl phthalate (DNOP), in urine samples. The PAEs in urine samples (500μL) were rapidly cleaned up from urines using polystyrene (PS) nanofibers packed micro-columns fitted on a PFSPE pretreatment device, which can process up to 12 samples simultaneously in 5min. Under optimum conditions, satisfied recovery and relative standard deviation values (RSDs) were in the range of 80.4-111.7% and 1.5-10.9%, respectively. The limits of detection (LOD) and the limits of quantification (LOQ) were ranged from 0.1 to 0.5ngmL and 0.5-2ngmL, respectively. The well controlled matrix effect was also evaluated by comparing the signal response of the pure PAEs standards dissolved in methanol with the signal response of PAEs in the urine matrix. This new method was successfully applied to determine four PAEs in urine samples of overweight and normal-weight children, and an association between phthalates in urines and obesity was observed. Thus, the method seems to be a useful tool for monitoring of the level of urinary phthalate esters and also to support an evidence for further reasearch of obesity.
在本文中,我们开发了一种快速且安全的方法,该方法基于填充纤维固相萃取(PFSPE)系统结合气相色谱 - 质谱联用技术,用于测定尿液样本中的四种邻苯二甲酸酯(PAEs),即邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2 - 乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)。尿液样本(500μL)中的PAEs使用安装在PFSPE预处理装置上的填充有聚苯乙烯(PS)纳米纤维的微柱从尿液中快速净化,该装置可在5分钟内同时处理多达12个样本。在最佳条件下,回收率和相对标准偏差值(RSDs)分别在80.4 - 111.7%和1.5 - 10.9%的范围内,令人满意。检测限(LOD)和定量限(LOQ)分别在0.1至0.5 ng/mL和0.5 - 2 ng/mL之间。还通过比较溶解在甲醇中的纯PAEs标准品的信号响应与尿液基质中PAEs的信号响应来评估良好控制的基质效应。这种新方法成功应用于测定超重和正常体重儿童尿液样本中的四种PAEs,并观察到尿液中的邻苯二甲酸酯与肥胖之间的关联。因此,该方法似乎是监测尿中邻苯二甲酸酯水平的有用工具,也为肥胖症的进一步研究提供了证据支持。