A survey of the occurrence of ochratoxin A in Madeira wines based on a modified QuEChERS extraction procedure combined with liquid chromatography–triple quadrupole tandem mass spectrometry

Fernandes, Paulo; Barros, Nelson; Câmara, José S.

doi:10.1016/j.foodres.2013.07.020

Cited by 44 publications

(19 citation statements)

References 47 publications

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“…The successful application of this method has been reported in many products, including cereals and their products [16], spices [17], nuts and seeds [18], Madeira wine [19], human breast milk [20], sesame butter [21], noodles [22], eggs [23], human biological fluids [24], and baby food [25]. In order to reduce the matrix effects (MEs), which can result in unsatisfactory recoveries, additional purification with sorbents such as octadecyl silica (C18), primary secondary amine (PSA), and graphitized carbon black (GCB) are commonly used.…”

Section: Introductionmentioning

confidence: 99%

QuEChERS Purification Combined with Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry for Simultaneous Quantification of 25 Mycotoxins in Cereals

Sun

Zhang

et al. 2016

Toxins

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A method based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) purification combined with ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS), was optimized for the simultaneous quantification of 25 mycotoxins in cereals. Samples were extracted with a solution containing 80% acetonitrile and 0.1% formic acid, and purified with QuEChERS before being separated by a C18 column. The mass spectrometry was conducted by using positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) models. The method gave good linear relations with regression coefficients ranging from 0.9950 to 0.9999. The detection limits ranged from 0.03 to 15.0 µg·kg−1, and the average recovery at three different concentrations ranged from 60.2% to 115.8%, with relative standard deviations (RSD%) varying from 0.7% to 19.6% for the 25 mycotoxins. The method is simple, rapid, accurate, and an improvement compared with the existing methods published so far.

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Section: Introductionmentioning

confidence: 99%

QuEChERS Purification Combined with Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry for Simultaneous Quantification of 25 Mycotoxins in Cereals

Sun

Zhang

et al. 2016

Toxins

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“…Such studies include quantification of low molecular weight polyphenols in vegetables (Silva et al 2012), polycyclic aromatic hydrocarbons (PAHs) in fish (Ramalhosa et al 2009), acrylamide in food (Mastovska and Lehotay 2006), veterinary drugs (Brondi et al 2013;de Souza et al 2013), mycotoxins in grains (Kokkonen and Jestoi 2009) dried fruits (Azaiez et al 2014) and cereal products (Cunha and Fernandes 2010;Vaclavik et al 2010;Zachariasova et al 2010;Soleiman et al 2011;Ferreira et al 2012) as well as in other matrices (Alvito et al 2010;Bertuzzi et al 2012;Fernandes et al 2013).…”

Section: Introductionmentioning

confidence: 99%

High-Throughput Analytical Strategy Based on Modified QuEChERS Extraction and Dispersive Solid-Phase Extraction Clean-up Followed by Liquid Chromatography-Triple-Quadrupole Tandem Mass Spectrometry for Quantification of Multiclass Mycotoxins in Cereals

et al. 2014

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A simple, reliable, efficient, selective and sensitive QuEChERS-based (quick, easy, cheap, effective, rugged and safe) sample preparation strategy, involving an initial partitioning step using acidified acetonitrile (ACN), MgSO 4 , NaCl and citrate buffer salts, combined with dispersive solidphase extraction (d-SPE) clean-up, is proposed for the simultaneous multiclass mycotoxins quantification, including aflatoxins, ochratoxins, fumonisins, trichothecenes and zearalenone, in cereals. The final clear extracts were concentrated under vacuum to near dryness and taken-up with the initial mobile phase (MeOH:H 2 O;70:30, v/v) previous to reversed-phase liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) analysis. Careful optimization of the LC-ESI-MS/MS parameters was achieved in order to attain a fast separation and increased sensitivity. The detection was carried out on a triplequadrupole tandem mass spectrometry (MS/MS) by electrospray ionization in positive ion mode (ESI + ) with multiple reaction monitoring (MRM). Tandem MS conditions were optimised in order to increase selectivity, selecting the best transitions (parent ion to quantifier and qualifier ions) for quantification and identification. The performance of the method was assessed and compared to European Commission (EC) Regulations, by studying the selectivity, specificity, limits of detection (LOD) and quantification (LOQ), linear dynamic range (LDR), matrix effect, accuracy, precision, and uncertainty. Good linearity (r 2 >0.9713) was achieved for all mycotoxins investigated, and LODs (S/N=3) and LOQs (S/ N=10) were below the tolerance levels of mycotoxins set by EC. Recoveries of the extraction process, obtained with different spiked concentrations, ranged from 72.9 to 120.6 %, with relative standard deviations (RSD) lower than 23.0 %. Only in 6 % of all combinations did the RSD values exceed 15 %. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of the solvent. The developed method was applied to evaluate the cooccurrence of multiclass mycotoxins in cereals collected at the importation points and consumer habitations at Madeira Island. Samples collected at importation points (15 wheat samples, 4 maize samples and 2 rice samples) showed the presence of DON in three wheat samples, and FB1 and HT-2 in one wheat sample. Three maize samples were detected with FB1 (two samples) and AFG 2 (one sample) whereas one rice sample was detected with ZEN. The results revealed the absence of target mycotoxins on the rice samples collected at consumer habitations. None of the studied cereal samples exceeded the maximum permissible limits or indicative levels set by the EC which means that the particular Madeira Island Electronic supplementary material The online version of this article (

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“…A method using ACN as extraction solvent, MgSO 4 and sodium acetate (as buffer) in a single step associated with ultra‐high performance liquid chromatography‐tandem mass spectrometry (UHPLC‐MS/MS) system was proposed and signal suppression as a matrix effect was observed . Additionally, another reported method for the analysis of OTA in wine was based on QuEChERS combined with liquid chromatography coupled to electrospray ionization‐tandem mass spectrometry (LC–ESI‐MS/MS) using a mixture of extraction solvents composed of acetonitrile and acetic acid (99:1), followed by extract clean‐up by means of dSPE . In this methodology, signal enhancement as a matrix effect was observed.…”

Section: Introductionmentioning

confidence: 99%

Assessment of ochratoxin A occurrence in Argentine red wines using a novel sensitive quechers‐solid phase extraction approach prior to ultra high performance liquid chromatography‐tandem mass spectrometry methodology

Mariño-Repizo

Gargantini²,

Manzano³

et al. 2016

J Sci Food Agric

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A survey of the occurrence of ochratoxin A in Madeira wines based on a modified QuEChERS extraction procedure combined with liquid chromatography–triple quadrupole tandem mass spectrometry

Cited by 44 publications

References 47 publications

QuEChERS Purification Combined with Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry for Simultaneous Quantification of 25 Mycotoxins in Cereals

QuEChERS Purification Combined with Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry for Simultaneous Quantification of 25 Mycotoxins in Cereals

High-Throughput Analytical Strategy Based on Modified QuEChERS Extraction and Dispersive Solid-Phase Extraction Clean-up Followed by Liquid Chromatography-Triple-Quadrupole Tandem Mass Spectrometry for Quantification of Multiclass Mycotoxins in Cereals

Assessment of ochratoxin A occurrence in Argentine red wines using a novel sensitive quechers‐solid phase extraction approach prior to ultra high performance liquid chromatography‐tandem mass spectrometry methodology

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