A multitoxin method for aflatoxins (AFs) and ochratoxin A (OTA) was modified and validated to analyze black pepper, colorífico, nutmeg, paprika, and turmeric. The method consisted of acetonitrile, NaHCO 3 and methanol extraction solution, multimycotoxin immunoaffinity column purification and isolation, reversed-phase liquid chromatography separation, and fluorescence detection. The limit of detection was <0.1 ng/g for AFs and OTA. Mean recoveries of added AFs ranged from 68 to 88% with relative standard deviation of repeatability (RSDr) values <15%; aflatoxin B 1 (AFB 1 ) from 69 to 92% with RSDr <17%; and OTA from 75 to 110% with RSDr <10% at spiked levels ranged from 8 to 40 ng/g for AFs, 4 to 20 ng/g for AFB 1 , and 4 to 20 ng/g for OTA, respectively. Recoveries of added aflatoxin G 2 were approximately 50% at spiked levels ranged from 1 to 5 ng/g. Recoveries of aflatoxin B 2 and aflatoxin G 1 were >70%. The linearity of the method for AFs ranged from 0.4 to 100 ng/g, for OTA from 0.2 to 40 ng/g with R 2 values exceeding 0.99. Results of a single laboratory validation study validated the performance of this method meeting the method acceptability criteria. No differences in toxin detection were determined in robustness testing in which minor changes were introduced to the method.
The incidence of aflatoxins and ochratoxin A in spices purchased from São Paulo State, Brazil was investigated. A total of 180 black pepper (Piper nigrum L.), colorífico (mixture of cornmeal or cassava flour with powdered annatto, Bixa orellana) ginger (Zingiber officinale Roscoe), nutmeg (Myristica fragrans), paprika (Capsicum annuum L.), and turmeric (Curcuma longa) were analyzed with a modified methods by using immunoaffinity column for clean-up and liquid chromatography/fluorescence detector for separation and quantification. Analytical methods were optimized for each spice, focusing mainly on the extraction step. OTA recoveries ranged from 65-102%. AFs recoveries were >70% except for AFG2. The average levels of AFs and OTA in black pepper, colorífico and turmeric samples were less than 2 ng/g. Twenty-five ginger samples (100%) contained OTA 0.10 -7.10 ng/g and 21 samples (84%) contained AFs 0.10 -9.55 ng/g. Twentynine nutmeg samples (100%) contained OTA 0.92 -65.49 ng/g and AFs 2.71 -48.67 ng/g. Thirty paprika samples (100%) contained OTA, 0.75 -147.18 ng/g and twenty-two samples (73%) contained AFs, 0.11 -14.92 ng/g. AFs and OTA in nutmeg and paprika could represent a food safety issue in Brazil.
We
have optimized the experimental conditions for the silver(I)-promoted oxidative
coupling of methyl <i>p</i>-coumarate (<b>I</b>) and methyl ferulate (<b>II</b>),
which is the most frequently used methodology to synthesize the bioactive dihydrobenzofuran
neolignans <b>1</b> ((±)-<i>trans</i>-dehydrodicoumarate dimethyl
ester) and <b>2</b> ((±)-<i>trans</i>-dehydrodiferulate
dimethyl ester). Most of the tested conditions affected the conversion (i.e.,
the consumption of <b>I</b> and <b>II</b>) and the selectivity (i.e., the
percentage of <b>I</b> and <b>II</b> that was converted into <b>1</b> and <b>2</b>,
respectively), so the optimized conditions were the conditions that afforded
the best balance between conversion and selectivity. Silver(I) oxide (0.5 eq) is the most efficient
oxidant agent amongst the silver(I) reagents that were tested to convert methyl
esters <b>I </b>and <b>II </b>into compounds <b>1</b> and <b>2</b>,
respectively. Acetonitrile, which has not yet been reported as a solvent for
this reaction, provided the best balance between conversion and selectivity,
besides being “greener” than other solvents that are more often employed (e.g.,
dichloromethane and benzene). Under the optimized conditions, the reaction time
decreased from 20 h to 4 h without significantly impacting the conversion and
selectivity. However, the relation between the results obtained by adding a radical
initiator (AIBN) or a radical inhibitor (isoquinoline) and the previously
reported involvement of radical intermediate species in the silver(I)-promoted
oxidative coupling of <b>I</b> and <b>II</b> is not clear and deserves further investigation.
O objetivo deste trabalho foi avaliar a presença de matérias estranhas em noz-moscada, (Myristica fragrans Houttuyn), cúrcuma (Curcuma longa Linnaeus), gengibre (Zingiber officinale Roscoe), colorífico (mistura de urucum [Bixa orellana Linnaeus] com fubá), pimenta-do-reino (Piper nigrum Linnaeus) e páprica (Capsicum annuum Linnaeus) conforme a legislação sanitária. Foram analisadas 180 amostras empregando os métodos preconizados pela AOAC International, de maio de 2018 a maio de 2020. A presença de ao menos uma matéria estranha foi observada em 80% das amostras. Pelos animais foram observados em todos os produtos e fragmentos de insetos foram encontrados na maioria das amostras. Ácaro, inseto inteiro, larva de inseto, bárbula e exúvia também foram encontrados, além de fibras sintéticas e fragmentos de microplásticos. Quanto à legislação, 47,8% das amostras estavam acima dos limites de tolerância, destas, 90,7% por conterem matérias estranhas indicativas de falhas na aplicação das boas práticas e 9,3% por matérias estranhas indicativas de risco à saúde. Os resultados obtidos denotam ineficiência da aplicação das medidas de boas práticas na cadeia produtiva e alertam para a intensificação da fiscalização direcionada ao cumprimento das normas sanitárias, além de provocarem a reflexão sobre a necessidade de alterações na legislação referente às matérias estranhas.
Especiarias são produtos constituídos de partes de espécies vegetais com importante valor alimentício e diversos benefícios para a saúde. O objetivo deste trabalho foi pesquisar adulterações na composição de cúrcuma (Curcuma longa Linnaeus), gengibre (Zingiber officinale Roscoe), noz-moscada (Myristica fragrans Houttuyn), páprica (Capsicum annuum Linnaeus), pimenta-do-reino (Piper nigrum Linnaeus) e colorífico (mistura de urucum, Bixa orellana Linnaeus, com fubá). Foram analisadas 180 amostras adquiridas em municípios do estado de São Paulo. A investigação dos elementos histológicos foi feita por microscopia óptica, a análise dos corantes por cromatografia em papel e a quantificação da bixina por cromatografia líquida de alta eficiência. Das amostras analisadas, 16,1% apresentaram elementos histológicos estranhos ao produto, sendo que nenhuma amostra apresentou corante orgânico artificial. A concentração de bixina nas amostras de colorífico variou entre 0,6 e 105,3 mg/100g, com média de 18,9 mg/100g e desvio padrão de 17,7 mg/100g. A avaliação microscópica revelou que a maioria das adulterações ocorre pela adição de amido de Zea mays. O colorífico não apresentou adulterações, porém foi constatada a necessidade de uma padronização da concentração de bixina. Este estudo demonstrou a necessidade da intensificação do monitoramento de adulterações em especiarias para que a comercialização de alimentos fidedignos seja garantida.
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