Lee M R, Yeh Y C, Hsiang W S, Chen C C
Department of Chemistry, National Chung-Hsing University, Taichung, Taiwan.
J Chromatogr B Biomed Sci Appl. 1998 Apr 10;707(1-2):91-7. doi: 10.1016/s0378-4347(97)00611-7.
This study investigated the feasibility of applying solid-phase microextraction (SPME) combined with gas chromatography-mass spectrometry to analyze chlorophenols in urine. The SPME experimental procedures to extract chlorophenols in urine were optimized with a polar polyacrylate coated fiber at pH 1, extraction time for 50 min and desorption in GC injector at 290 degrees C for 2 min. The linearity was obtained with a precision below 10% R.S.D. for the studied chlorophenols in a wide range from 0.1 to 100 microg/l. In addition, sample extraction by SPME was used to estimate the detection limits of chlorophenols in urine, with selected ion monitoring of GC-MS operated in the electron impact mode and negative chemical ionization mode. Detection limits were obtained at the low ng/l levels. The application of the methods to the determination of chlorophenols in real samples was tested by analyzing urine samples of sawmill workers. The chlorophenols were found in workers, the urinary concentration ranging from 0.02 microg/l (PCP) to 1.56 microg/l (2,4-DCP) depending on chlorophenols. The results show that trace chlorophenols have been detected with SPME-GC-MS in the workers of sawmill where chlorophenol-containing anti-stain agents had been previously used.
本研究探讨了应用固相微萃取(SPME)结合气相色谱 - 质谱联用技术分析尿液中氯酚的可行性。采用极性聚丙烯酸酯涂层纤维,在pH 1条件下,萃取时间为50分钟,并在气相色谱进样口于290℃解吸2分钟,对尿液中氯酚的固相微萃取实验程序进行了优化。在所研究的氯酚浓度范围为0.1至100微克/升时,线性关系良好,相对标准偏差(R.S.D.)低于10%。此外,利用固相微萃取进行样品萃取,通过在电子轰击模式和负化学电离模式下运行的气相色谱 - 质谱联用仪的选择离子监测,估算尿液中氯酚的检测限。检测限可达纳克/升水平。通过分析锯木厂工人的尿液样本,测试了该方法在实际样品中氯酚测定的应用。在工人尿液中发现了氯酚,根据氯酚种类不同,尿液浓度范围为0.02微克/升(五氯苯酚)至1.56微克/升(2,4 - 二氯苯酚)。结果表明,在先前使用含氯酚防污剂的锯木厂工人中,利用固相微萃取 - 气相色谱 - 质谱联用技术检测到了痕量氯酚。