期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1218, 期 14, 页码 1815-1821出版社
ELSEVIER
DOI: 10.1016/j.chroma.2011.02.010
关键词
Microwave assisted extraction; Dispersive liquid-liquid microextraction; Gas chromatography-mass spectrometry; Nitrosamines; Meat products
资金
- Spanish MICINN [CTQ2009-08267/BQU]
- Departamento de Formacion del Personal Academico de la Universidad Centroccidental Lisandro Alvarado (Venezuela)
Microwave-assisted extraction (MAE) and dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) were evaluated for use in the extraction and preconcentration of volatile nitrosamines in meat products. Parameters affecting MAE, such as the extraction solvent used, and DLLME, including the nature and volume of the extracting and disperser solvents, extraction time, salt addition and centrifugation time, were optimized. In the MAE method, 0.25 g of sample mass was extracted in 10 mL NaOH (0.05 M) in a closed-vessel system. For DLLME, 1.5 mL of methanol (disperser solvent) containing 20 mu L of carbon tetrachloride (extraction solvent) was rapidly injected by syringe into 5 inL of the sample extract solution (previously adjusted to pH 6), thereby forming a cloudy solution. Phase separation was performed by centrifugation, and a volume of 3 mu L of the sedimented phase was analyzed by GC-MS. The enrichment factors provided by DLLME varied from 220 to 342 for N-nitrosodiethylamine and N-nitrosopiperidine, respectively. The matrix effect was evaluated for different samples, and it was concluded that sample quantification can be carried out by aqueous calibration. Under the optimized conditions, detection limits ranged from 0.003 to 0.014 ng mL(-1) for NPIP and NMEA, respectively (0.12-0.56 ng g(-1) in the meat products). (C) 2011 Elsevier B.V. All rights reserved.
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