Determination of N-nitrosopiperidine in beers by liquid chromatography with reductive amperometric detection at a hanging mercury drop electrode

Goicolea, M. Aránzazu; Balugera, Zuriñe Gómez de; Portela, M.J.; Barrio, Ramón J.

doi:10.1016/0003-2670(94)00443-p

Cited by 7 publications

(3 citation statements)

References 19 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…Neste sentido, Goicolea et al 12 utilizaram um eletrodo de mercúrio como detector eletroquímico, associado à cromatografia líquida de alta eficiência, para a determinação de N-nitrosopiperidina (NPIP) em cervejas. A fase móvel utilizada foi metanol-acetonitrila-tampão fosfato pH 3,5 (57:38:5 v/v/v) com o detector operando no modo de corrente direta (DC) a potencial de -1250 mV.…”

Section: Introductionunclassified

Comportamento eletroquímico da N-nitrosotiazolidina ácido carboxílico sobre eletrodos de ouro e mercúrio

Codognoto¹,

Reyes²,

Winter³

et al. 2008

Quím. Nova

View full text Add to dashboard Cite

Recebido em 11/4/07; aceito em 17/12/07; publicado na web em 31/7/08 ELECTROCHEMICAL BEHAVIOR OF N-NITROSOTHIAZOLIDINE CARBOXILIC ACID ON GOLD AND MERCURY ELECTRODES. The electrochemical behavior of N-nitrosothiazolidine carboxylic acid (NTAC) on gold and hanging mercury electrodes, using the cyclic and square wave voltammetries, was studied. Whereas NTAC suffer reduction in a single step on the mercury electrode, two peaks appears on the cyclic voltammograms on the gold electrode, one anodic peak overlaying the gold oxide process at 1.2 V and one cathodic peak at -0.41 V vs Ag/AgCl, KCl 3.0 mol L -1. The cathodic peak depends on the previous oxidation of NTAC at the electrode surface, presents irreversible and adsorption controlled characteristics and it is suitable for quantitative purposes.Keywords: N-nitrosothiazolidine carboxylic acid; voltammetry; gold electrode. introduçãoOs compostos N-nitrosos, e em particular as N-nitrosaminas, são considerados potentes carcinógenos, além de apresentarem ação teratogênica e mutagênica em animais de laboratório. As nitrosaminas podem ser encontradas nas mais diversas matrizes, entre essas, alimentos, solos, água, ar, pesticidas, cigarros, produtos de borracha e cosméticos. Nos alimentos podem ser encontradas em diversos produtos, principalmente nos industrializados, como presunto, salsicha, salame e outros produtos cárneos, nos quais são formadas a partir de precursores nitrosáveis do próprio alimento e de agentes nitrosantes. [1][2][3] É importante ressaltar que, devido ao nitrato poder ser reduzido a nitrito na cavidade bucal e, sendo a faixa ótima de pH para a formação de N-nitrosaminas semelhante àquela encontrada no estômago do homem após ingestão de alimentos, a formação de N-nitrosaminas in vivo torna-se um assunto de extrema importância. 4,5 Para fins analíticos, as N-nitrosaminas são divididas em voláteis e não voláteis. As diferenças nas propriedades químicas e fisicoquímicas desses compostos dificultam o estabelecimento de métodos analíticos de aplicação geral.6 Todavia, os métodos cromatográficos têm sido os mais utilizados na determinação de nitrosaminas em matrizes diversas, onde a cromatografia líquida de alta eficiência e a cromatografia gasosa tem sido empregadas para a determinação das nitrosaminas não voláteis e voláteis, respectivamente. Os detectores mais utilizados em ambas as técnicas têm sido o de quimiluminescência (TEA -Thermal Energy Analyzer), uma vez que esse é seletivo para compostos que contêm o grupo N-nitroso 7-9 e o de massas. 10,11Entretanto, as técnicas cromatográficas associadas ao detector de quimiluminescência ou ao espectrômetro de massa requerem alto investimento inicial e, em função disto, poucas indústrias no Brasil controlam seus produtos quanto à presença de nitrosaminas. O Brasil tem inúmeros alimentos típicos, assim como situações diferenciadas de processamento de alimentos que propiciam a formação de N-nitrosaminas (processamento caseiro de bacon, elaboração e comercialização de lingüiças de preparo tipo caseiro). Desta fo...

show abstract

Section: Introductionunclassified

Comportamento eletroquímico da N-nitrosotiazolidina ácido carboxílico sobre eletrodos de ouro e mercúrio

Codognoto¹,

Reyes²,

Winter³

et al. 2008

Quím. Nova

View full text Add to dashboard Cite

show abstract

“…In conclusion and as a summary, the proposed method affords the simultaneous determination of seven NAms in beverages. By contrast, most existing methods can only determine one (NDMA or NPIR) ,,,,, or two N -nitrosamines (NDMA and NDEA or NDMA and NPIR) , in beer; a few allow several N -nitrosamines to be determined in alcoholic beverages ,, .…”

Section: Resultsmentioning

confidence: 99%

“…The determination of NAms in beverages has been carried out by gas chromatography using nitrogen–phosphorus detection (NPD) , thermal energy analyzer , , or mass spectrometry (MS) detection , . Liquid chromatography with fluorescence , chemiluminiscence , photoconductivic , amperometric , mass spectrometric , or colorimetric detection has also been employed for this purpose. Recently, micellar electrokinetic chromatography with diode array detection has also been used for the determination of NAms in sausages .…”

Section: Introductionmentioning

confidence: 99%

Gas Chromatographic Determination of N-Nitrosamines in Beverages Following Automatic Solid-Phase Extraction

Jurado‐Sánchez

Ballesteros

Gallego

2007

J. Agric. Food Chem.

View full text Add to dashboard Cite

A semiautomatic method for the determination of seven N-nitrosamines in beverages by gas chromatography with nitrogen-phosphorus detection is proposed. Beverage samples are aspirated into a solid-phase extraction module for preconcentration and cleanup. The influence of the experimental conditions was examined by using various sorbents among which LiChrolut EN was found to provide quantitative elution and the highest preconcentration factors of all. The proposed method is sensitive, with limits of detection between 7 and 33 ng/kg, and precise, with relative standard deviations from 4.3% to 6.0%. The recoveries of N-nitrosamines from beverage samples spiked with 0.5 or 1 microg/kg concentrations of these compounds ranged from 95% to 102%. The method was successfully applied to the determination of residues of the studied N-nitrosamines in beverages including beer, wine, liquor, whisky, cognac, rum, vodka, grape juice, cider, tonic water, and soft drinks. The analytes were only detected in beer samples, positives being confirmed by gas chromatography coupled with impact ionization mass spectrometry.

show abstract

Determination of simazine and cymoxanil in soils by microwave-assisted solvent extraction and HPLC with reductive amperometrical detection

Sabando

Balugera²,

Goicolea

et al. 2002

Chromatographia

View full text Add to dashboard Cite

SummaryA microwave-assisted extraction (MAE) method was optimized for the herbicide simazine and the fungicide cymoxanil in soil samples. The experimental variables that affect MAE, such as temperature, extraction time and solvent volume, were studied. It was concluded that these pesticides could be efficiently extracted from soil samples in a microwave oven with 10 mL of acetonitrile at 90 ~ for 5 min The analysis of extracts has been carried out by high performance liquid chromatography with amperometric reductive detection (HPLC-ED). The detector, equipped with a hanging mercury drop electrode (HMDE), operated in direct current mode at-1.2 Vvs Ag/AgCI, when a mobile phase consisting of phosphate buffer-acetonitrile (95:5, v/v) was used. The procedure developed involving MAE and HPLC-ED provided detectability in soil samples of 30 I~g Kg 1, acceptable recoveries (range 82.3-100.3%) and RSDs of lower than 5% for cymoxanil and simazine.

show abstract

Determination of N-nitrosopiperidine in beers by liquid chromatography with reductive amperometric detection at a hanging mercury drop electrode

Cited by 7 publications

References 19 publications

Comportamento eletroquímico da N-nitrosotiazolidina ácido carboxílico sobre eletrodos de ouro e mercúrio

Comportamento eletroquímico da N-nitrosotiazolidina ácido carboxílico sobre eletrodos de ouro e mercúrio

Gas Chromatographic Determination of N-Nitrosamines in Beverages Following Automatic Solid-Phase Extraction

Determination of simazine and cymoxanil in soils by microwave-assisted solvent extraction and HPLC with reductive amperometrical detection

Contact Info

Product

Resources

About