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顶空固相微萃取后气相色谱/质谱法对全血中萘、芴和蒽的简单分析

Simple analysis of naphthalene, fluorene, and anthracene in whole blood by gas chromatography/mass spectrometry after headspace-solid phase microextraction.

作者信息

Akdoğan Hatice Ardag

机构信息

Pamukkale University, Faculty of Arts and Sciences, Department of Biochemistry, 20017 Denizli, Turkey.

出版信息

J AOAC Int. 2011 Nov-Dec;94(6):1891-5. doi: 10.5740/jaoacint.11-124.

DOI:10.5740/jaoacint.11-124
PMID:22320097
Abstract

A simple and sensitive method for the simultaneous analysis of naphthalene, fluorene, and anthracene in whole blood was developed using headspace-solid-phase microextraction (SPME) and GC/MS. A 0.5 g whole blood sample, 5 microL naphthalene, fluorene, and anthracene (50 microg/mL) as spiked standards, and 0.5 mL sodium hydroxide were placed into a 12 mL vial and sealed rapidly. The vial was immediately heated to 70 degrees C in an aluminium block heater, the needle of the SPME device was inserted through the septum of the vial, and the extraction fiber was exposed to the headspace for 15 min. Afterwards, the compounds extracted by the fiber were desorbed simultaneously by exposing the fiber in the gas chromatograph injection port. No interferences were found, and the time for analysis was about 30 min for one sample. This method was applied to a suicide case in which the victim ingested naphthalene, fluorene, and anthracene.

摘要

采用顶空-固相微萃取(SPME)和气相色谱/质谱联用技术,建立了一种简单、灵敏的同时分析全血中萘、芴和蒽的方法。将0.5 g全血样品、5 μL萘、芴和蒽(50 μg/mL)作为加标标准品以及0.5 mL氢氧化钠置于一个12 mL的小瓶中,并迅速密封。小瓶立即在铝块加热器中加热至70℃,将SPME装置的针穿过小瓶的隔膜插入,使萃取纤维暴露于顶空15分钟。之后,将纤维在气相色谱进样口中暴露,使纤维萃取的化合物同时解吸。未发现干扰,一个样品的分析时间约为30分钟。该方法应用于一起受害者摄入萘、芴和蒽的自杀案件。

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