期刊
TALANTA
卷 83, 期 5, 页码 1562-1567出版社
ELSEVIER
DOI: 10.1016/j.talanta.2010.11.060
关键词
Screening; Microextraction in packed sorbent; Capillary liquid chromatography; Fluorescence detection; Heterocyclic aromatic amines; Urine
资金
- Ministry of Science and innovation (MICINN)
- JJCC Castilla-La Mancha [CTQ2010-15027, PCC08-0015-0722]
A rapid and simple procedure for the direct screening of urine samples is described. The method involves microextraction in a packed sorbent (MEPS) that is on-line coupled to a capillary liquid chromatograph with fluorimetric detection. The overall arrangement works as a screening/confirmatory system for monitoring non-polar heterocyclic aromatic amines (HAAs) in urine samples. This configuration allows the selective retention of HAAs from urine on a C-18 MEPS cartridge integrated in the needle of a micro-well plate autosampler. Retained HAAs were eluted with methanol/water (90:10, v/v) and directly injected into the fluorimetric detector. This screening method provides a yes/no binary response that may require confirmation. The samples for which the concentration of HAAs was close to or above the established threshold limit (30 ng mL(-1)) were subjected to capillary liquid chromatography (CLC) for confirmation purposes. A mobile phase of acetonitrile and triethylamine (25 mM) at pH 2.5, through a gradient of composition at a flow rate of 20 mu L min(-1). resulted in good separations between the analytes in less than 11 min. This confirmation method allowed the determination of the analytes in the 10-100 ng mL(-1) range for harmane and norharmane and from 20 to 200 ng mL(-1) for 3-amino-1,4-dimethyl-5H-pyrido-[4,3-b] indole (Trp-P-1), 3-amino-1-methyl-5H-pyrido-[4,3-b] indole (Trp-P-2), 2-amino-9H-pyrido-[2,3-b] indole (A alpha C) and 2-amino-3-methyl-9H-pyrido-[2,3-b] indole (MeA alpha C), with relative standard deviation (RSD) values between 2.12% and 3.73%, and limits of detection between 1.6 and 5.6 ng mL(-1) for all the HAAs. (C) 2010 Elsevier B.V. All rights reserved.
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