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苯并[a]芘和二苯并[a,h]蒽在色谱馏分中的共洗脱及其在烟草提取物中的明确测定 激光激发时间分辨的 Shpol'skii 光谱法。

On the co-elution of benzo[]pyrene and dibenzo[,]pyrene in chromatographic fractions and their unambiguous determination in tobacco extracts laser-excited time resolved Shpol'skii spectroscopy.

机构信息

Department of Chemistry, University of Central Florida, 4000 Central Florida Blvd., Physical Science Room 255, Orlando, FL, 3281-2366, USA.

出版信息

Anal Methods. 2023 Apr 27;15(16):1959-1968. doi: 10.1039/d2ay02064e.

DOI:10.1039/d2ay02064e
PMID:37017264
Abstract

High performance liquid chromatography is widely used for the analysis of polycyclic aromatic hydrocarbons in a wide variety of samples. Of particular concern are benzo[]pyrene and dibenzo[,]pyrene, two of the most toxic polycyclic aromatic hydrocarbons ever tested. Under EPA method 610, these two compounds co-elute with almost identical retention times. Our studies demonstrate the feasibility of directly determining them in a chromatographic fraction without further separation. Their unambiguous determination is based on spectral and lifetime information with a two-step experimental procedure consisting of the evaporation of the chromatographic fraction followed by the dissolution of the residue with microliters of -octane. With the aid of a 77 K fiber optic probe, limits of detection at the parts-per-billion concentration level (ng mL) are obtained from the microliter sample laser excited time resolved Shpol'skii spectroscopy. This approach is then applied to the analysis of benzo[]pyrene and dibenzo[,]pyrene in tobacco extracts.

摘要

高效液相色谱法广泛用于分析各种样品中的多环芳烃。特别值得关注的是苯并[]芘和二苯并[,]芘,这两种多环芳烃是迄今为止测试过的最具毒性的多环芳烃之一。根据 EPA 方法 610,这两种化合物在几乎相同的保留时间下共同洗脱。我们的研究表明,无需进一步分离即可直接在色谱馏分中直接确定它们的可行性。它们的明确确定基于光谱和寿命信息,实验步骤分为两步,包括色谱馏分的蒸发,然后用微升正辛烷溶解残渣。借助于 77 K 光纤探头,从微升样品中获得纳克毫升的十亿分之几浓度水平(ng mL)的检测限激光激发时间分辨光谱。然后将该方法应用于烟草提取物中苯并[]芘和二苯并[,]芘的分析。

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