Method validation for mycotoxin determinations in food and feedstuffs

Boenke, Achim

doi:10.1016/s0165-9936(97)00084-8

Cited by 8 publications

(1 citation statement)

References 27 publications

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“…The monitoring of aflatoxins -which are present in food and feed usually inmg/kg -depends on precise, reliable and efficient methods for their accurate determination [10].…”

Section: -Introduçãomentioning

confidence: 99%

Determining aflatoxins B1, B2, G1 and G2 in maize using florisil clean up with thin layer chromatography and visual and densitometric quantification

Castro¹,

Vargas²

2001

Ciênc. Tecnol. Aliment.

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1 Recebido para publicação em 25/01/00. Aceito para publicação em 07/05/01. 2 ministério da agricultura e do abastecimento -laboratório de controle de qualidade e segurança alimentar/LAV/MG. Av. Raja Gabaglia, 245, BH, MG, Brasil, CEP 30380-090. email:gena@cdlnet.com.br; * A quem a correspondência deve ser enviada. SUMMARYA method for determining aflatoxins B 1 (AFB 1 ), B 2 (AFB 2 ),G 1 (AFG 1 ) andG 2 (AFG 2 ) in maize with florisil clean up was optimised aiming at one-dimensional thin layer chromatography (TLC) analysis with visual and densitometric quantification. Aflatoxins were extracted with chloroform: water (30:1, v/v), purified through florisil cartridges, separated on TLC plate, detected and quantified by visual and densitometric analysis. The in-house method performance characteristics were determined by using spiked, naturally contaminated maize samples, and certified reference material. The mean recoveries for aflatoxins were 94.2, 81.9, 93.5 and 97.3% in the range of 1.0 to 242 µg/kg for AFB 1 , 0.3 to 85mg/kg for AFB 2 , 0.6 to 148mg/kg for AFG 1 and 0.6 to 140mg/kg for AFG 2 , respectively. The correlation values between visual and densitometric analysis for spiked samples were higher than 0.99 for AFB 1 , AFB 2 , AFG 1 and 0.98 for AFG 2 . The mean relative standard deviations (RSD) for spiked samples were 16.2, 20.6, 12.8 and 16.9% for AFB 1 , AFB 2 , AFG 1 and AFG 2 , respectively. The RSD of the method for naturally contaminated sample (n = 5) was 16.8% for AFB 1 and 27.2% for AFB 2 . The limits of detection of the method (LD) were 0.2, 0.1, 0.1 and 0.1mg/kg and the limits of quantification (LQ) were 1.0, 0.3, 0.6 and 0.6mg/kg for AFB 1 , AFB 2 , AFG 1 and AFG 2 , respectively. (218 words) Keywords: aflatoxins; florisil; maize; thin-layer chromatography (TLC); densitometry. RESUMODETERMINAÇÃO DE AFLATOXINAS B 1 , B 2 ,G 1 EG 2 EM MI-LHO UTILIZANDO PURIFICAÇÃO COM FLORISIL, SEPARA-ÇÃO POR CROMATOGRAFIA EM CAMADA DELGADA E QUANTIFICAÇÃO VISUAL E DENSITOMÉTRICA. Um méto-do para determinação de aflatoxinas B 1 (AFB 1 ), B 2 (AFB 2 ),G 1 (AFG 1 ) eG 2 (AFG 2 ) em milho utilizando florisil na etapa de purificação foi otimizado com vistas a cromatografia em camada delgada (CCD) unidimensional com quantificação visual e densitométrica. As aflatoxinas foram extraídas com solução de clorofórmio: água (30:1, v/v), purificada em cartuchos de florisil, separada em placas cromatográfica de sílicagel, detectadas e quantificadas por análise visual e densitométrica. As características do método foram determinadas utilizando amostras de milho natural e artificialmente contaminadas e material de referência certificado. Os valores de recuperação média para cada aflatoxina obtidos na faixa de 1,0 a 242 µg/kg para AFB 1 , 0,3 a 85mg/kg para AFB 2 , 0,6 a 148 mg/kg para AFG 1 e 0,6 a 140mg/ kg para AFG 2 foram respectivamente 94,2; 81,9 93,5 e 97,3% por análise densitométrica. As correlações obtidas entre análi-se visual e densitométrica para amostras artificialmente contaminadas foram maiores que 0,99 para AFB 1 ...

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“…The monitoring of aflatoxins -which are present in food and feed usually inmg/kg -depends on precise, reliable and efficient methods for their accurate determination [10].…”

Section: -Introduçãomentioning

confidence: 99%

Determining aflatoxins B1, B2, G1 and G2 in maize using florisil clean up with thin layer chromatography and visual and densitometric quantification

Castro¹,

Vargas²

2001

Ciênc. Tecnol. Aliment.

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Analytical methods for the determination of aflatoxins in various food matrices at concentrations regarding the limits set in european regulations: development, characteristics, limits

2000

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Methods for the determination of aflatoxins in paprika, peanut butter, pistachio paste, fig paste and baby food were developed. The methods employ an immunoaffinity cleanup step and reversed-phase liquid chromatography. All steps of the analysis were tested for their suitability for all matrices with focus on method robustness, simplicity, toxicology, environment, and user friendliness. Extraction procedures, chromatographic separation and post column derivatisation techniques were elaborated for this purpose. The methods were statistically validated in collaborative trials at currently established legal limits for aflatoxins and are in the process for adoption as official methods by CEN and AOAC.

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Aflatoxin contamination in insect damaged seeds of horsegram under storage

2005

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Studies on one of the protein rich pulses, horsegram (Dolichos biflorus L.) were carried out to know how far these low risk pulses are free from aflatoxin contamination under severe insect infestation in storage. A total of 150 stored seed samples of horsegram were analyzed for the presence of aflatoxins by collecting 25 samples each of undamaged and insect damaged seeds of all the three varieties (PDM-1, PHG-1 and HG-96). More than 33% of insect damaged seed samples were contaminated with aflatoxin B1 and B2, whereas less than 8% of the undamaged seed samples contain only low levels of aflatoxin B2. Higher levels of aflatoxin B1 (up to 130 μg/kg) were reported in insect damaged seed samples of all the three varieties under study. The levels of aflatoxin B2 were always lower than aflatoxin B1 of the corresponding seed samples with insect damage. Aflatoxin B1 was reported in both the undamaged and insect damaged seed samples of all the three varieties of horsegram. It is evident from the varietal response studies that PDM-1 and HG-96 varieties of horsegram are highly vulnerable to aflatoxin contamination whereas, PHG-1 variety is relatively less susceptible to it. In general, insect infestation leads to increase in fungal invasion (including aflatoxigenic fungi) and this further enhances the levels of aflatoxin contamination in horsegram seeds.

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Method validation for mycotoxin determinations in food and feedstuffs

Cited by 8 publications

References 27 publications

Determining aflatoxins B1, B2, G1 and G2 in maize using florisil clean up with thin layer chromatography and visual and densitometric quantification

Determining aflatoxins B1, B2, G1 and G2 in maize using florisil clean up with thin layer chromatography and visual and densitometric quantification

Analytical methods for the determination of aflatoxins in various food matrices at concentrations regarding the limits set in european regulations: development, characteristics, limits

Aflatoxin contamination in insect damaged seeds of horsegram under storage

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