Método QuEChERS para determinação de ocratoxina a e citrinina em arroz e farelo de arroz

Hackbart, Helen C. dos S.; Souza, Michele Moraes de; Scaglioni, Priscila Tessmer; Prímel, Ednei Gilberto; Garda‐Buffon, Jaqueline; Badiale‐Furlong, Eliana

doi:10.1590/s0100-40422012000900006

Cited by 4 publications

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References 30 publications

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“…Anastassíades e colaboradores em 2003, introduziram um método de preparo de amostra descrito como rápido, fácil, de baixo custo, efetivo, robusto e seguro, denominado QuEChERS, o qual inicialmente foi destinado à análise de resíduos de pesticidas em frutas e vegetais (QUEIROZ et al, 2012). Devido a sua versatilidade, o método foi adaptado para diferentes classes de micotoxinas conforme (HACKBART et al, 2012e LIU et al, 2014. Mostrando-se promissor para extração em diversas matrizes.…”

Section: Técnica De Preparo De Amostras Quechers Versão Originalunclassified

“…Devido à dificuldade de realizar a remoção de coextrativos nas amostras de vegetais, os extratos obtidos ainda podem conter grandes quantidades de componentes da matriz que podem afetar negativamente o sistema de detecção dependendo do método de extração adotado (LIU et al, 2014). Para superar algumas das limitações dos métodos existentes, há uma necessidade de desenvolver métodos de extração e limpeza para a determinação simultânea de várias micotoxinas com altas recuperações e minimizando os efeitos da matriz de amostras (HACKBART et al, 2012).…”

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Isolamento, caracterização e determinação de alcaloides triptoquialanina A e triptoquialanina C produzidos pelo fungo Penicillium digitatum durante infecção no hospedeiro citros

Araújo¹

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Fungi, are responsible for large post-harvest losses in various commodities. In particular, Penicillium digitatum, which is responsible for up to 90% of the total losses to the Brazilian citrus crop in the post-harvest period. During infection in the citrus host, the phytopathogen P.digitatum synthesizes tryptoquialanines A and C alkaloids in vivo, which could represent a problem for the world population, since mycotoxins produced by fungi in general are notoriously toxic. The objective of this project were to isolate, characterize and develop and validate an analytical method to determination of tryptoquialanines A and C during the infection of the fungus P.digitatum in orange (layers: epicarp, mesocarp and endocarp), evaluating the level of diffusion of these mycotoxins in different stages of infection. Purification of the standards was performed by chromatographic techniques and the compounds were characterized by NMR ( 1 H, 13 C, HSQC, HMBC) and Liquid Chromatographic coupled to High Resolution Mass Spectrometry (LC-HR-MS) techniques. The purified alkaloid standards were then used to develop and validate the analytical method which employed the QuEChERS extraction method, modified with the aid of experimental planning and the quantification of the analytes was carried out by Liquid Chromatography coupled to Tandem Mass Spectrometry (LC-MS/MS). The linearity obtained was 5 -400 μg/kg with r > 0.99 for tryptoquialanines A and C. The limits of detection (LOD) and quantification (LOQ) were 5 μg/kg and 10 μg/kg, with the exception of the TC compound in the epicarp extract, where the LQ was 25 μg/kg. The recoveries between 58 and 101%, with relative standard deviations (RSDs) ≤ 12% showed the accuracy of the method. The presence of the tryptoquialanines A and C was observed in different levels of infection of the orange, showing the diffusion of the metabolites occurs only from the intermediate stage of the infection.In addition, the presence of the compounds in the epicarp layer (blank), which was in direct contact for 48 hours with infected orange, showed the contamination process among oranges by the alkaloids, after this exposure period. Tryptoquialanines compounds A and C did not demonstrate antiproliferative and cytotoxicity abilities in the tests performed (HeLa, HUVEC and K-562), which suggests absence of activities for the analyzed cells.

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Section: Técnica De Preparo De Amostras Quechers Versão Originalunclassified

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Isolamento, caracterização e determinação de alcaloides triptoquialanina A e triptoquialanina C produzidos pelo fungo Penicillium digitatum durante infecção no hospedeiro citros

Araújo¹

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Principal components analysis: An innovative approach to establish interferences in ochratoxin A detection

Kupski

Badiale‐Furlong

2015

Food Chemistry

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This work aimed to establish an innovative approach to evaluate the effect of cereals composition on ochratoxin A extraction by multivariate analysis. Principal components analysis was applied to identify the effect of major matrix components on the recovery of ochratoxin A by QuEChERS method using HPTLC and HPLC, and to validate the method for ochratoxin A determination in wheat flour by HPLC. The matrices rice bran, wheat bran and wheat flour were characterized for their physical and chemical attributes. The ochratoxin A recovery in these matrices was highly influenced (R=0.99) by the sugar content of the matrix, while the lipids content showed a minor interference (R=0.29). From these data, the QuEChERS method was standardized for extracting ochratoxin A from flour using 1% ACN:water (2:1) as extraction solvent and dried magnesium sulfate and sodium chloride as salts. The recovery values ranged from 97.6% to 105%. The validated method was applied to evaluate natural occurrence of ochratoxin A in 20 wheat flour samples, which were contaminated with ochratoxin A levels in the range of 0.22-0.85 μg kg(-1).

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Evaluation of the TLC quantification method and occurrence of deoxynivalenol in wheat flour of southern Brazil

Rocha

Oliveira

Badiale‐Furlong

et al. 2017

Food Additives & Contaminants: Part A

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The study evaluated a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction method for use with a TLC quantification procedure for deoxynivalenol (DON). It also surveyed DON occurrence in wheat flour from the southern region of Brazil. Forty-eight wheat flour samples were analysed, divided into 2 different harvest lots, each consisting of 24 different brands. The detection and quantification limits of the method were 30 and 100 ng of DON on the TLC plate. The various concentrations of DON presented high linearity (R = 0.99). A negative matrix effect (-28%) of the wheat flour was verified, with suppression of the chromatographic signal of DON, and 80.2-105.4% recovery. The TLC method was reliable for DON evaluation, with a coefficient of variation of less than 10%. High-performance liquid chromatography of lot 2 samples confirmed the presence of DON in all samples identified DON-positive by the TLC technique. Of the 48 wheat flour samples in lots 1 and 2 analysed by TLC, 33.3 and 45.8% of the samples respectively were above the Brazilian legislation limit. Correlations were observed between the water activity and DON content, and between the fungal count and moisture content of the wheat flours.

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Método QuEChERS para determinação de ocratoxina a e citrinina em arroz e farelo de arroz

Cited by 4 publications

References 30 publications

Isolamento, caracterização e determinação de alcaloides triptoquialanina A e triptoquialanina C produzidos pelo fungo Penicillium digitatum durante infecção no hospedeiro citros

Isolamento, caracterização e determinação de alcaloides triptoquialanina A e triptoquialanina C produzidos pelo fungo Penicillium digitatum durante infecção no hospedeiro citros

Principal components analysis: An innovative approach to establish interferences in ochratoxin A detection

Evaluation of the TLC quantification method and occurrence of deoxynivalenol in wheat flour of southern Brazil

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