52a Reunião Anual da Sociedade Brasileira de Zootecnia Zootecnia: Otimizando Recursos e Potencialidades Belo Horizonte – MG, 19 a 23 de Julho de 2015 Stability Oxidative evaluation of Flaxseed Cake (Linum usitatissimum) by means of indices of acidity and peróxidos1 Jessyca Caroline Rocha Ribas2, Marina Tolentino Marinho3, Adriana de Souza Martins4, Maria de Fátima dos Santos Ribeiro5, Erica Machado6 1 Part of the final paper of Animal Science Course at the State University of Ponta Grossa - UEPG Student of Animal Science, Graduate Program - UEM, Maringá-PR, Brazil. E-mail: [email protected] 3 Teacher, Department of Food Engineering, State University of Ponta Grossa - UEPG. Email: [email protected] 4 Teacher, Department of Animal Science at the State University of Ponta Grossa - UEPG. Email: [email protected] 5 Researcher of Plant Science and Agro-Energy Program Agronomic Institute of Paraná – IAPAR. Email: [email protected] 6 PhD Student, Animal Science Graduate Program – UEM, Maringá – PR, Brazil. E-mail: [email protected] 2 Resumo: Avaliou-se a estabilidade oxidativa do óleo da torta de linhaça em teste de oxidação acelerada, utilizando métodos clássicos (acidez e peróxidos). A torta foi obtida por meio de prensagem a frio, com prensa experimental. A estabilidade oxidativa foi determinada pelo método em estufa (oxidação acelerada), diariamente, durante nove dias, em estufa a 65º C. Sob estas condições, cada dia na estufa equivale a um mês à temperatura ambiente. As variáveis acidez e peróxido foram submetidas à análise de variância utilizando-se o teste de Fisher.O índice de acidez aumentou com o tempo de armazenamento da torta, porém, manteve-se abaixo do limite máximo estabelecido pela ANVISA. O índice de peróxidos apresentou oscilações durante o processo de oxidação acelerada. O óleo da torta de linhaça submetido aos testes de acidez e peróxido manteve uma estabilidade oxidativa satisfatória, podendo ser armazenada por um período de nove meses. Palavras–chave: ácidos graxos, óleo, oxidação lipídica, palatabilidade Abstract: Was evaluated the oxidative stability of oil of cake flaxseed in accelerated oxidation test, using classical methods (acidity and peroxides). The cake was obtained by cold pressing, with experimental press. Oxidative stability was determined by the method oven (accelerated oxidation) daily, for nine days in an incubator at 65ºC. Under these conditions one day in the oven was equivalent a month at room temperature. The variables acidity and peroxide were subjected to analysis of variance using the Fisher test. The acid value increased with storage time of the pie, but remained below the ceiling set by ANVISA. The peroxide index showed variations during the accelerated oxidation process. The oil of linseed cake subjected to acidity and peroxide tests maintained a satisfactory oxidative stability and can be stored for a period of nine months. Keywords: fat acids, oil, oxidative stability, palatability Introduction Flaxseed (Linum usitatissimum) is an oilseed plant produced on a large scale in Canada, where it is widely used in dairy cows to produce milk enriched. In food, the increase in consumption of flaxseed has been associated with decreased cardiovascular disease, prostate cancer and breast cancer, osteoporosis and menopausal symptoms. The cake is a co-product of the oil extraction of oil plants through pressing, and has a higher oil content in relation to meal. The oil contained in the cake increases the energy content of the diet and, when consumed by animals, may amend this fatty acid profile in meat/milk products, making them healthier for human consumption. Flaxseed contains polyunsaturated fatty acids, however, the disadvantage of working with oleaginous materials is the possibility of oxidizing, reducing the nutritional quality of the food due to the degradation of fat soluble vitamins and essential fatty acids, besides modifying the odor and taste food. The animals, in general, tend to decrease the consumption of food with modified organoleptic properties. Therefore, the objective was to evaluate the oxidative stability of oil linseed cake from the classical methods: acid values and peroxides. Material e Methods The experiment was conducted in Food Analysis Laboratory of the State University of Ponta Grossa (UEPG). Flaxseed cake was obtained from a small-scale seed press Scott Tech model ERT-60. The flaxeed cake used in this experiment presented 17% of ether extract. The oxidative stability of linseed cake was evaluated by the method oven (accelerated oxidation), also known as a Schaal method. According to the method, 9 trays of cake flaxseed crushed containing 100g of cake was ________________________________________________________________________________________________________________________________________________ Página - 1 - de 3 52a Reunião Anual da Sociedade Brasileira de Zootecnia Zootecnia: Otimizando Recursos e Potencialidades Belo Horizonte – MG, 19 a 23 de Julho de 2015 thermally stressed at 65 ° C in an oven and analyzed for acidity and peroxide over a period of nine days, one at a time, including day 0 (zero), which comprises cake sample at room temperature. Thus, 10 samples were analyzed during the evaluation period. Daily, at 9: 00min were collected 90 g sample of the cake for oil extraction for determination of acidity and peroxide, the extraction was performed in triplicate, using 30 g cake per sample. The oil extraction of cake was performed according to the Bligh-Dyer method (BLIGH and Dyer, 1959). Under conditions of heat stress by storing in an oven, the every day in the oven equals one month at room temperature (Almeida et al., 2011). When detecting the first signal or rancidity change in peroxide value, was determined the induction period, measured in days. The acid value was determined according to the methodology of the AOCS Ca 5A-40 (1990), expressed as mg KOH per gram of sample and calculated according to the equation: IA = [V x f x 56,1]/m, where IA = index acidity; V = volume of NaOH solution 0.01 mol L-1in the sample spent in the titration (ml); f= correction factor of NaOH solution; 56.1 = equivalent weight basis of KOH; m = sample weight in grams. The index of peroxides was obtained according to AOCS Cd 8-53 (1990), expressed in milliequivalents peroxide per kg of the sample obtained by the following equation: IP = [(B-A) x N x f x 1000]/m; where PV = peroxide value; B = volume of sodium 0.01 mol.L-1spent thiosulfate solution in the blank titration (ml); A = volume of sodium 0.01 mol.L-1solution in spent thiosulfate titration of the sample (ml); C = concentration of sodium thiosulphate solution; f = factor of the sodium thiosulfate solution; m = sample weight in grams. The variables acidity and peroxide were subjected to analysis of variance (ANOVA) using Fisher's post hoc test for difference between means, the 1% significance level. Results and Discussion The acid values and peroxide of samples subjected to the accelerated oxidative stability test are described in Table 1. Table 1: Index of Acid (AI) and peroxides (PI) from oil samples of flakseed cake, submitted to accelerated test analysis in function of evaluation day Day 0 1 2 3 4 5 6 7 8 9 AI (mg KOH/g ) 1.80±0.02e 2.06±0.44de 2.38±0.01cd 2.38±0.01cd 2.47±0.21cd 2.78±0.16bc 3.01±0.19b 3.18±0.07b 3.69±0.18a 3.77±0.12a PI (mEq peroxide/kg) 0.99±0.01c 1.96±0.03b 2.01±0.01b 2.97±0.03ª 2.97±0.09ª 2.97±0.03ª 3.51±0.70ª 2.00±0.01b 1.48±-0.71bc 1.47±0.65bc Means followed by different letters at the same column, differ by the Fisher test (P<0.01). The acid number indicates the condition of oils and fats. It is defined as the number of milligrams of potassium hydroxide required to neutralize the free fatty acids of 1.0 g of the sample (ITB, 2008). Therefore, the higher the acid value, the greater the deterioration of the product. This rate was increased (P <0.01) with the progressive deterioration of thermal oil. Ruminant rations containing oil may have stability issues due to factors such as ambient temperature, humidity and storage because they favor the lipid oxidation process. The oxidative deterioration of lipids can cause rancid flavor in food, reducing consumption by animals. According to ANVISA, cold pressed oils are unrefined and having a maximum acid number of 4.0 mg KOH / g. Therefore, the results of flaxseed cake acid value are within the standards recommended by ANVISA (BRAZIL, 2005). Thus, it appears that the linseed cake storage for nine months (one day in a greenhouse was a month at room temperature) does not impair its properties, and therefore will not interfere in the intake by the animals. Peroxide Index (PI) is a way to detect rancidity of fat. According to Souza (2003) their use should be limited only to the initial stage of oxidation, since the peroxides have poor stability, it decomposes into intermediate products (aldehydes, alcohols, ketones and hydrocarbons). The oxidation of oils can form undesirable products in foods such as peroxides and reactive intermediates, the so-called free radicals, which affect the quality of feed by the reduced palatability and digestibility of food, harming animal performance. The results showed oscillations in the peroxide value, where, at first moment (0 to 6 days of accelerated oxidation), increase was observed in the peroxide level and then (7th to 9th day of oxidation), had progressive ________________________________________________________________________________________________________________________________________________ Página - 2 - de 3 52a Reunião Anual da Sociedade Brasileira de Zootecnia Zootecnia: Otimizando Recursos e Potencialidades Belo Horizonte – MG, 19 a 23 de Julho de 2015 decrease, reaching 1.47 meq peroxide / kg (9 days in accelerated oxidation process). For peroxide value, ANVISA establishes the maximum limit of 15 mEq / kg, so the linseed cake also lie within the recommended levels for this index. However, it is emphasized that the low level of peroxides in the sample does not represent good oxidative stability guarantee and may mean pronounced change. Conclusions The oil of linseed cake subjected to acidity and peroxide tests maintained a satisfactory oxidative stability, be within the standards recommended by ANVISA. Flaxseed cake can be stored for a period of nine months, without compromising its oxidative stability. References Almeida, C. G.; Rodrigues, C.; Demiate, I. M.; Simões, D. R.; Tolentino, M. C.; 2011. Apoio técnico à implantação de uma unidade processadora de derivados de tomate no município de reserva – processamento e análises. In: 9° CONEX: Conversando sobre extensão. UEPG, Paraná. AOCS – American Oil Chemists’ Society. 1988.Official methods analysis: 3rd ed., Champaign, Illinois, USA. Bligh, E. G.; Dyer, W. J. 1959. A rapid method of total lipid extraction and purification.p. 911-917. In: Canadian Journal of Biochemistry and Physiology. v. 37, n. 8. Brasil. 2005. Resolução nº270, de 23 de setembro de 2005. Disponível em: <http://elegis.anvisa.gov.br/leisref/public/showAct.php?id=18829&word>. Acesso em: outubro de 2013. IAL - Instituto Adolfo Lutz (São Paulo). 2008.Métodos Físico-químicos para Análise deAlimentos. São Paulo:Instituto Adolfo Lutz, p. 1020. Souza, A. V. C. 2003. Avaliação da Qualidade e Valor Nutricional de Óleos e gorduras. .Net, São Paulo, Seção Artigos do Mês. Disponível em: <http://www.polinutri.com.br/conteudo_artigos_anteriores_agosto0 3.htm>. Acesso em: 2 maio de 2008. ________________________________________________________________________________________________________________________________________________ Página - 3 - de 3