Optimisation of the derivatisation reaction and subsequent headspace solid-phase microextraction method for the direct determination of chlorophenols in red wine

Martínez-Uruñuela, Almudena; González-Sáiz, J.M.; Pizarro, Consuelo

doi:10.1016/j.chroma.2004.07.026

Cited by 42 publications

(21 citation statements)

References 44 publications

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“…In contrast, for red wine, quantification of analytes is not possible by direct calibration with hydroalcoholic solution, so matrix-matched standards must be used. Although Martínez-Uruaeuela et al [30] reported that the sample matrix does not interfere in the HS-SPME for the analysis of chlorophenols in red and synthetic wines, our results are in agreement with those published in other papers, which highlight the influence of working with different wine matrices [25,40]. In a more recent work [32], significant differences were observed when comparing the slopes for calibration curves prepared with red and synthetic wine and the authors propose the application of the MHS-SPME procedure which leads to a complete extraction of the analytes and, consequently, matrix effect was avoided.…”

Section: Matrix Effect: Comparison Between Synthetic and Real Winesmentioning

confidence: 97%

“…In the SPME analysis of the chlorophenols from water samples, a PDMS fibre was selected [9]. Martínez-Uruaeuela et al [30] proposed either PDMS or PDMS-divinylbenzene (PDMS-DVB) or polyacrylate (PA) for the determination of chlorophenols contained in wine samples. In a previous work [31], we demonstrated the usefulness of PDMS fibre for the extraction of chlorinated phenols from hydroalcoholic cork macerates and preliminary results for wine were also presented.…”

Section: Selection Of Hs-spme Parametersmentioning

confidence: 99%

“…While SPME applications for TCA analysis in wines have been commonly reported [23 -29], its chlorophenolic precursors have been studied very little. To the best of our knowledge, only Martínez-Uruaeuela et al [30] reported the use of this methodology for the determination of chlorophenols in red wine. Additionally, in a previous work [31], we studied the analysis of chlorophenols from cork macerates and white wine samples and SPME was used following a step by step optimization.…”

Section: Introductionmentioning

confidence: 97%

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Assessment of the matrix effect on the headspace solid‐phase microextraction (HS‐SPME) analysis of chlorophenols in wines

Insa¹,

Besalú²,

Salvadó³

et al. 2007

J of Separation Science

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In this paper, we propose a comparative study to check the matrix effect on the extraction of three chlorophenols, 2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol and pentachlorophenol, direct precursors of 2,4,6-trichloroanisole, in synthetic and commercial wines (white and red wines). A rapid, simple and sensitive methodology based on solid-phase microextraction (SPME) and GC with electron capture detection (GC-ECD) and mass spectrometric detection (GC-MS) was developed and the variables affecting the extraction process (temperature, time and salt content) were examined employing a factorial design at two levels. Since GC-ECD does not allow the clear identification of target analytes in white wine, owing to overlapped interferences, GC-MS/MS was used for subsequent examinations. Calibration curves were constructed in synthetic, white and red wine. Significant differences between the slopes of synthetic and red wine, with the exception of TCP, were observed. Analytical parameters were evaluated and satisfactory results were obtained, showing the usefulness of the headspace SPME (HS-SPME) method for determining chlorophenolic compounds in wines.

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Section: Matrix Effect: Comparison Between Synthetic and Real Winesmentioning

confidence: 97%

Section: Selection Of Hs-spme Parametersmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 97%

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Assessment of the matrix effect on the headspace solid‐phase microextraction (HS‐SPME) analysis of chlorophenols in wines

Insa¹,

Besalú²,

Salvadó³

et al. 2007

J of Separation Science

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show abstract

“…Currently, the research has been highly focused on the field of the environment, especially the contamination of CPs in water (De Morais, Stoichev, Basto, & Vasconcelos,2012). However, the migration and transformation of chlorophenols to foods drew more attention during very recent years (Maggi, Zalacain, Mazzoleni, Alonso, & Salinas, 2008;Martínez-Uruñuela, Rodríguez, Cela, González-Sáiz, & Pizarro, 2005; Martínez-Uruñuela, González-Sáiz, & Pizarro, 2004;Campillo, Viñas, Cacho, Peñalver,& Hernández-Córdoba, 2010;Röhrig, & Meisch, 2000;Diserens, 2001;Veningerová, Prachar, Kovacicova, & Uhnák, 1997;Campillo, Penalver, & Hernández-Córdoba, 2006).…”

Section: Introductionmentioning

confidence: 97%

Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid–liquid microextraction as a pretreatment method followed by high-performance liquid chromatography

Fan

Cao

2015

Food Chemistry

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In-situ ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) method was developed as a pretreatment method for the detection of six chlorophenols (CPs) in honey samples. The hydrophobic ionic liquid [C4MIM][NTf2], formed in-situ by the hydrophilic ionic liquid [C4MIM][BF4] and the ion exchange reagent LiNTf2 was used as the microextractant solvent of CPs from honey sample. Then the enriched analytes were back-extracted into 40 μL of 0.14 M NaOH solution and finally subjected to analysis by high-performance liquid chromatography. The method showed low limit of detection of CPs, 0.8-3.2 μg/L and high enrichment factor, 34-65 with the recoveries range from 91.60% to 114.33%. The method is simple, rapid, environmentally friendly and with high extraction efficiency.

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“…They also have substantial applications in agriculture as herbicides, insecticides and fungicides. Due to their moderate bioaccumulation and high toxicity, they can cause serious health hazards, which depend on the degree of chlorination and the position of the chlorine atoms [1,2], and most of them are determined as priority contaminant by the US Environmental Protection Agency [3]. Therefore, developing reliable, sensitive and simple methods is of great interest for the determination of phenols in environmental, food, and biological samples.…”

Section: Introductionmentioning

confidence: 99%

Headspace single drop and hollow fiber liquid phase microextractions for HPLC determination of phenols

Hu²,

Hou

2008

J of Separation Science

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Two methods based on headspace single drop microextraction (HS-SDME) and headspace hollow fiber liquid phase microextraction (HS-HF-LPME) were developed and critically compared with HPLC-UV determination of phenols (including phenol (Ph), 2-chlorophenol (CP), 2,4-dichlorophenol (DCP) and 2,4,6-trichlorophenol (TCP)) in this paper. The significant parameters affecting the extraction efficiency of the target analytes in both extraction modes were studied and the optimal extraction conditions were established. Under the optimal conditions, the detection limits (S/N = 3) for Ph, CP, DCP and TCP obtained by HS-SDME-HPLC-UV and HS-HF-LPME-HPLC-UV were 2.1, 0.2, 0.8,1.1 ng/mL and 4.2, 0.4, 0.4, 0.4 ng/mL with enrichment factors of 15.8, 198.9, 159.7, 194.8 and 9.2, 149.9, 301.9, 411.1, respectively. The RSDs obtained by HS-SDME-HPLC-UV and HS-HF-LPME-HPLC-UV were 3.7, 4.0, 9.8, 6.7% and 6.3, 3.6, 3.1, 4.8% for Ph, CP, DCP and TCP, respectively. Both extraction modes have a comparable analytical performance, but HS-HF-LPME was more robust than HS-SDME, while HS-SDME was simpler than HS-HF-LPME. The two headspace microextraction modes were applied for HPLC-UV determination of target phenols in water, honey and toner samples, and the determined values obtained by both techniques were in good agreement with each other.

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Optimisation of the derivatisation reaction and subsequent headspace solid-phase microextraction method for the direct determination of chlorophenols in red wine

Cited by 42 publications

References 44 publications

Assessment of the matrix effect on the headspace solid‐phase microextraction (HS‐SPME) analysis of chlorophenols in wines

Assessment of the matrix effect on the headspace solid‐phase microextraction (HS‐SPME) analysis of chlorophenols in wines

Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid–liquid microextraction as a pretreatment method followed by high-performance liquid chromatography

Headspace single drop and hollow fiber liquid phase microextractions for HPLC determination of phenols

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