Department of Chemistry, 4000 Central Florida Blvd, University of Central Florida, Orlando, FL 32816-2366, USA. korin
Talanta. 2011 Sep 30;85(4):1805-11. doi: 10.1016/j.talanta.2011.07.009. Epub 2011 Jul 14.
Urine analysis of monohydroxy metabolites is recognized as an accurate assessment of human exposure to polycyclic aromatic hydrocarbons. Despite the sophisticated arsenal of analytical tools, monitoring of monohydroxy metabolites via simple, cost effective and direct methods of analysis still remains a challenge. This article evaluates the analytical potential of solid-phase extraction room-temperature fluorescence spectroscopy for the problem at hand. Extraction membranes serve the dual purpose of sample pre-concentration and solid substrate for RTF measurements. The potential of our proposition is demonstrated with the analysis of 2-hydroxy-fluorene, 1-hydroxy-pyrene, 3-hydroxy-benzo[a]pyrene and 9-hydroxy-phenanthrene in synthetic urine samples. Signal reproducibility is improved with the aid of a sample holder specifically designed for the manual optimization of luminescence signals. Background correction of solid substrates is carried out with the aid of Asymmetric Least Squares. Recovery values for the studied metabolites varied from 99.0 ± 1.2% (3-hydroxy-benzo[a]pyrene) to 99.9 ± 0.05% (1-hydroxy-pyrene). With only 10 mL of urine sample, the limits of detection varied from 57 pg mL(-1) (2-hydroxy-fluorene) to 2 pg mL(-1) (1-hydroxy-pyrene). Additional figures of merit include a simple experimental procedure for routine screening of numerous samples and compatibility with portable instrumentation for field analysis. Because of the non-destructive nature of fluorescence measurements, membranes can be brought to the lab for subsequent elution and confirmation of compounds via high-resolution techniques.
尿液中单羟基代谢物的分析被认为是评估人体多环芳烃暴露的一种准确方法。尽管有复杂的分析工具,但通过简单、经济高效和直接的分析方法来监测单羟基代谢物仍然是一个挑战。本文评估了固相萃取-室温荧光光谱法在这一问题上的分析潜力。萃取膜具有样品预浓缩和 RTF 测量固体基质的双重作用。我们的方法通过分析合成尿液样品中的 2-羟基芴、1-羟基芘、3-羟基苯并[a]芘和 9-羟基菲来证明其潜力。通过专门设计的用于手动优化荧光信号的样品支架,提高了信号重现性。采用非对称最小二乘法对固体基质进行背景校正。研究代谢物的回收率从 99.0 ± 1.2%(3-羟基苯并[a]芘)到 99.9 ± 0.05%(1-羟基芘)不等。仅用 10 mL 尿液样品,检测限从 57 pg mL(-1)(2-羟基芴)到 2 pg mL(-1)(1-羟基芘)不等。其他重要指标包括用于常规筛选大量样品的简单实验程序以及与便携式仪器的兼容性,用于现场分析。由于荧光测量是非破坏性的,因此可以将膜带到实验室,通过高分辨率技术进行后续洗脱和化合物确认。