Determination of 2,4,6-Trichloroanisole and 2,4,6-Tribromoanisole in Wine Using Microextraction in Packed Syringe and Gas Chromatography−Mass Spectrometry

Jönsson, Sofia; Hagberg, Jessika; Bavel, Bert van

doi:10.1021/jf800230y

Cited by 38 publications

(13 citation statements)

References 51 publications

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“…After extraction the bed volume can be washed with solvent before elution of the target compounds. However, until now, the application of this methodology to wine volatile compounds is limited to the analysis of the taints 2,4,6-tricholoanisole and 2,4,6-tribromoanisole (Jönsson et al, 2008).…”

Section: Adsorptive-based Techniquesmentioning

confidence: 99%

Application of Gas Chromatography on the Evaluation of Grape and Wine Aroma in Atlantic Viticulture (NW Iberian Peninsula)

Vilanova¹,

Oliveira²

2012

Gas Chromatography in Plant Science, Wine Technology, Toxicology and Some Specific Applications

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Section: Adsorptive-based Techniquesmentioning

confidence: 99%

Application of Gas Chromatography on the Evaluation of Grape and Wine Aroma in Atlantic Viticulture (NW Iberian Peninsula)

Vilanova¹,

Oliveira²

2012

Gas Chromatography in Plant Science, Wine Technology, Toxicology and Some Specific Applications

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“…CAR/PDMS extracts with high efficiency ethyl hexanoate (6), p-cymene (9), (Z)-3-hexen-1-ol (13), 2-acetylfuran (24), whereas PDMS is more indicated to extract 1-dodecene (19), decanal (22), ␣-ionol (43), diethyl malate (46), and octanoic (47), tetradecanoic (55), and hexadecanoic acids (56). PA …”

Section: Hs-spme Analysismentioning

confidence: 99%

“…Moreover, MEPS applied to the analysis of wine volatile and semi-volatile constituents has been poorly studied [46]. The study presented herein represents a first approach of the analysis of wine volatile profile using MEPS.…”

Section: Introductionmentioning

confidence: 99%

Effectiveness of high-throughput miniaturized sorbent- and solid phase microextraction techniques combined with gas chromatography–mass spectrometry analysis for a rapid screening of volatile and semi-volatile composition of wines—A comparative study

Mendes¹,

Gonçalves²,

Câmara³

2012

Talanta

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a b s t r a c tIn this study the feasibility of different extraction procedures was evaluated in order to test their potential for the extraction of the volatile (VOCs) and semi-volatile constituents (SVOCs) from wines. In this sense, and before they could be analysed by gas chromatography-quadrupole first stage masss spectrometry (GC-qMS), three different high-throughput miniaturized (ad)sorptive extraction techniques, based on solid phase extraction (SPE), microextraction by packed sorbents (MEPS) and solid phase microextraction (SPME), were studied for the first time together, for the extraction step. To achieve the most complete volatile and semi-volatile signature, distinct SPE (LiChrolut EN, Poropak Q, Styrene-Divinylbenzene and Amberlite XAD-2) and MEPS (C 2 , C 8 , C 18 , Silica and M1 (mixed C 8 -SCX)) sorbent materials, and different SPME fibre coatings (PA, PDMS, PEG, DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS), were tested and compared. All the extraction techniques were followed by GC-qMS analysis, which allowed the identification of up to 103 VOCs and SVOCs, distributed by distinct chemical families: higher alcohols, esters, fatty acids, carbonyl compounds and furan compounds. Mass spectra, standard compounds and retention index were used for identification purposes.SPE technique, using LiChrolut EN as sorbent (SPE LiChrolut EN ), was the most efficient method allowing for the identification of 78 VOCs and SVOCs, 63 and 19 more than MEPS and SPME techniques, respectively. In MEPS technique the best results in terms of number of extractable/identified compounds and total peak areas of volatile and semi-volatile fraction, were obtained by using C 8 resin whereas DVB/CAR/PDMS was revealed the most efficient SPME coating to extract VOCs and SVOCs from Bual wine. Diethyl malate (18.8 ± 3.2%) was the main component found in wine SPE LiChrolut EN extracts followed by ethyl succinate (13.5 ± 5.3%), 3-methyl-1-butanol (13.2 ± 1.7%), and 2-phenylethanol (11.2 ± 9.9%), while in SPME DVB/CAR/PDMS technique 3-methyl-1-butanol (43.3 ± 0.6%) followed by diethyl succinate (18.9 ± 1.6%), and 2-furfural (10.4 ± 0.4%), are the major compounds. The major VOCs and SVOCs isolated by MEPS C8 were 3-methyl-1-butanol (26.8 ± 0.6%, from wine total volatile fraction), diethyl succinate (24.9 ± 0.8%), and diethyl malate (16.3 ± 0.9%). Regardless of the extraction technique, the highest extraction efficiency corresponds to esters and higher alcohols and the lowest to fatty acids.Despite some drawbacks associated with the SPE procedure such as the use of organic solvents, the time-consuming and tedious sampling procedure, it was observed that SPE LiChrolut EN , revealed to be the most effective technique allowing the extraction of a higher number of compounds (78) rather than the other extraction techniques studied.

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“…7,8 The MEPS technique has been used to extract a wide range of analytes from different matrices, such as biological fluids (plasma, blood, and urine), [7][8][9][10][11][12][13][14][15][16][17][18][19][20] water, 21,22 hair 23 and wine. 24,25 In the areas of food analysis, several published applications describe MEPS for the analysis of aflatoxin B2 and M2 metabolite trace analysis in milk, mycotoxin trace analysis in cereal, atrazine in cereal, and sulfonamide trace analysis in meat. 26 A key factor in MEPS is that the solvent volume employed in the elution of analytes during the extraction process is of a suitable order of magnitude to be injected directly into an LC or GC system.…”

mentioning

confidence: 99%

Microextraction in packed sorbent for determination of sulfonamides in egg samples by liquid chromatography and spectrophotometric detection

Salami¹,

Queiroz²

2011

J. Braz. Chem. Soc.

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O presente trabalho descreve a aplicação bem sucedida da microextração em sorvente empacotado e cromatografia líquida com detecção de arranjo de diodos (MEPS/LC-DAD) para a determinação simultânea das sulfonamidas (sulfacetamida, sulfadiazina, sulfatiazol, sulfametazina sulfametoxipiridazina e sulfametoxazol) em amostras de ovos. As variáveis MEPS (pH da amostra, número de ciclos aspirar/dispensar, força iônica e procedimento de dessorção) foram otimizados para aumentar a sensibilidade analítica do método. O método apresentou linearidade na faixa de concentração de 30 ng g -1 (limite de quantificação, LOQ) a 300 ng g -1. Este valor de LOQ é inferior ao limite máximo de resíduo (LMR) preconizado para sulfonamidas em amostras de ovos (100 µg kg -1 ). As taxas de recuperação foram adequadas para todos os analitos (> 94%), bem como os dados de precisão inter-ensaio, com coeficientes de variação inferiores a 10%. Com base na validação analítica, a metodologia MEPS/LC é adequada para a determinação de sulfonamidas em amostras de ovos.The present work describes a successful application of microextraction packed sorbent and liquid chromatography with diode array detection (MEPS/LC-DAD) for simultaneous determination of the sulfonamides (sulfacetamide, sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypiridazine and sulfamethoxazole) in egg samples. The MEPS variables (pH of the sample, draw-eject cycles, ionic strength, and desorption procedure) were optimized, in order to improve the sensitivity of the proposed method. The method was shown to be linear at concentrations ranging from 30 ng g -1 (limit of quantification, LOQ) to 300 ng g -1 . This LOQ value is lower than those established as the maximum residue limit (MRL) for egg samples (100 µg kg -1 ). The accuracy values were adequate for all analytes (> 94%), as well as the inter-day precision data, with coefficient of variation lower than 10%. On the basis of analytical validation, the MEPS/LC methodology has been shown to be a promising alternative for analysis of sulfonamides in egg samples. Keywords: MEPS, sulfonamides, liquid chromatography, egg IntroductionSulfonamides (SAs) are a group of synthetic antibiotics that have played an important role as effective chemotherapeutics in bacterial and protozoan infections in veterinary medicine practice. Subtherapeutic doses of more than ten SAs are routinely used in food-producing animals for prophylactic and growth-promoting purposes. SAs residues could be potentially toxic to aquatic organisms and humans because of their carcinogenic potency and possible antibiotic resistance. [1][2][3][4] There are no sulfonamides approved for use in laying hens. The use of veterinary drugs for medicinal purposes in laying hens could result in violative drug residues in food meant for human consumption. Of all the marketed SAs, only sulfamethazine and sulfadimethoxine have been approved for use in chickens. Furthermore, this approval extends to broilers only, not laying hens. 4,5 To safeguard human health, many countries ...

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Determination of 2,4,6-Trichloroanisole and 2,4,6-Tribromoanisole in Wine Using Microextraction in Packed Syringe and Gas Chromatography−Mass Spectrometry

Cited by 38 publications

References 51 publications

Application of Gas Chromatography on the Evaluation of Grape and Wine Aroma in Atlantic Viticulture (NW Iberian Peninsula)

Application of Gas Chromatography on the Evaluation of Grape and Wine Aroma in Atlantic Viticulture (NW Iberian Peninsula)

Effectiveness of high-throughput miniaturized sorbent- and solid phase microextraction techniques combined with gas chromatography–mass spectrometry analysis for a rapid screening of volatile and semi-volatile composition of wines—A comparative study

Microextraction in packed sorbent for determination of sulfonamides in egg samples by liquid chromatography and spectrophotometric detection

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