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Thermoanalytical Study and Characterization of Native Starches of Paraná Pine Seeds (Araucaria Angustiofolia, Bert O

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Thermoanalytical Study and Characterization of Native Starches of Paraná Pine Seeds (Araucaria Angustiofolia, Bert O EQ01-AF:MODELO-AF 7/20/09 10:08 PM Página 7 www.scielo.br/eq www.ecletica.iq.unesp.br Volume 34, número 1, 2009 Thermoanalytical study and characterization of native starches of Paraná pine seeds (Araucaria angustiofolia, Bert O. Ktze) and European chestnut seeds (Castanea sativa, Mill) S. C. W. Bicudo 1, I. M. Demiate 1, G. Bannach 1, L. G. Lacerda 2, M. A. S. Carvalho Filho 3, M. Ionashiro 4 and E. Schnitzler 1* 1Universidade Estadual de Ponta Grossa – UEPG. Av. Carlos Cavalcanti, 4748. CEP 84030-000 – Ponta Grossa – PR, Brazil. 2Universidade Federal do Paraná – UFPR. Curitiba – PR. Brazil 3Universidade Positivo – Curitiba – PR. Brazil 4Universidade Estadual Paulista – UNESP. Instituto de Química de Araraquara - Araraquara – SP - Brazil *[email protected] Abstract: Starch is the most important carbohydrate storage in plants. It is a raw material with diverse botanical origins, and is used by the food, paper, chemical, pharmaceutical, textile and other industries. In this work, native starches of Paraná pine seeds (pinhão) ( Araucaria angustiofolia , Bert O. Ktze) and european chestnut seeds ( Castanea sativa , Mill) were studied by thermoanalytical techniques: thermo - gravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC), as well as X-ray powder patterns diffractometry. Apparent and total amylose content was also determined. Keywords: Starch; gelatinization; thermal analysis; enthalpy. Introduction acterized by a limited shelf-life because of their high water activity and sugar contents [5]. The conifer, “Paraná pine tree” European chestnut trees spread all over (Araucaria angustiofolia, Bert O. Ktze), grows the world produce wood and chestnuts that have naturally in forest of Brazil (south), Paraguay, considerable economical value. In Brazil, howev - Chile and Argentina. It seeds, named “pinhão”, er, they are not products of economic interest; are eaten by mammals and birds; cooked or roast - trees are growth for their landscape qualities in ed, are consumed as traditional high-caloric food many farms and also in some public squares, during winter by humans [1, 2]. “Pinhão” (Paraná mainly in Southern Region [6]. pine seeds), is a source of complex carbohy - Starch, a semi crystalline polymer, is com - drates: starch ( ~ 36%), proteins ( ~ 3%), lipids ( ~ posed of two polysaccharides: amylose and amy - 1%), soluble sugars ( ~2.4%), beyond fiber, min - lopectin. Amylose, a mostly linear chain, typical - erals and phenolic compounds (< 0.2 mg %) [3]. ly consists up to 3000 glucose molecules inter - “Chestnut” seeds ( Castanea sativa , Mill.), connected primarily by a a-1,4 glycosidic link - is multipurpose specie that is cultivated for tim - ages and is reported to contain a few branched ber, nut, tannin and contributes positively to the networks [7]. Amylopectin is a large branched forestry landscape [4]. It seeds chestnuts are char - polymer with linkages of a-1,4 that serve as the Ecl. Quím., São Paulo, 34(1): 7-12, 2009 7 EQ01-AF:MODELO-AF 7/20/09 10:08 PM Página 8 backbone and a-1,6 bridges that serve as branch - described in the literature [1]. After this procedure, ing points [8]. the obtained starches were kept in a desiccator over Thermogravimetry (TG) can be helpful to anhydrous calcium chloride until constant mass. show the behavior of starch granules when heat - TG and DTA curves were recorded using a ing leads to depolymerization [11; 17]. simultaneous TG 60 system (Shimadzu) under a Starch, when heated in the presence of 100 mL min -1 air flow and a 10 oC min -1 heating excess water, undergoes the order to disorder rate of. The initial sample mass was about 9 mg. phase transition known as gelatinization over a Alumina crucibles were used for the TG and DTA temperature range characteristic of the starch experiments. DSC curves were recorded using a source. This phase transition is associated with DSC 60 (Shimadzu) under an air flow of 100 mL diffusion of water into the granule, water uptake min -1 , heating rate of 5 oC min -1 . Sealed alu - by the amorphous background region, hydration minum crucibles were used and the studies were and radial swelling of the starch granules, loss of carried out in order to study the gelatinization birefringence, loss of crystalline order, uptake of process, according the following conditions: 1 st heat, uncoiling and dissociation of double helices condition - a 4:1 (water:starch w/w) mixture was in the crystalline regions and amylase leaching prepared and left for two hours stirring in order to [9; 10; 15]. The gelatinization process, which is a equilibrate the moisture content. With a micro- function of the starch : water ratio, can be studied pipette 10 mL of this emulsion was transferred for by differential scanning calorimetry (DSC). an aluminum crucible, which was sealed and car - In recent years, substantial efforts have ried out in order to study the gelatinization been made to obtain starches from non-conven - process. The 2 nd condition was: a 10:1 tional sources and to study their functional, rheo - (water:starch w/w) was prepared directly by logical and physicochemical properties [13 - 15]. weighting 1,0 mg of each starch and up to this Starch is used in the food industry to mass 10 mL of water was added; the aluminum impart functional properties, and to modify food crucible was sealed and after one hour a new texture and consistency. Both the amount of DSC curve was realized. The 3 rd condition was: a starch and its type are critical for the texture of a 5:1 (water:starch w/w) was prepared directly by given product [14 - 16]. weighting 2,0 mg of each starch and up to this Efforts have been made to find native mass 10 mL of water was added; the aluminum starches with the necessary properties for the crucible was sealed and after one hour a new food industry (syneresis, transparency, DSC curve was realized. freeze/thaw stability), with no chemical or genet - X-ray diffraction powder patterns were ic modification. In this way, the knowledge about obtained by using a D-5000 X Ray diffractometer the characteristics of different native starches is (Siemens), with CuK a radiation ( l = 1.544 Å) of great importance to select the most suitable and a setting of 40kV and 20 mA. starch for a specific application [2]. Total and apparent amylose were deter - Since pinhão and european chestnut were mined according the technique described by good sources of starch and they have a large poten - Hoower and Ratnayake [12], in a spectrophotome - tial for commercial use, the objective of this work ter (Shimadzu UV mini 1240) at l = 600 nm. was to evaluate some thermoanalytical and chem - The procedure for apparent amylose con - ical, characteristics of these isolated starches. tent was: starch sample (20 mg) was dissolved in 90% of dimethylsulfoxide (8 ml) in 10 ml at screw-cap reaction vials. The content of the vial Experimental was vigorously mixed for 20 min and then heated in a water bath (with intermittent shaking) at 85 oC Both seeds were acquired in the local mar - for 15 min. The vial was then cooled to ambient ket at Ponta Grossa – Pr – Brazil. All chemicals temperature, and the content diluted with water to used were analytical reagent grade. Extraction and 25 mL in a volumetric flask. An aliquot (1.0 mL) purification of each starch were performed as of the diluted solution was mixed with water (40 8 Ecl. Quím., São Paulo, 34(1): 7-12, 2009 EQ01-AF:MODELO-AF 7/20/09 10:08 PM Página 9 -3 ml) and 5mL of I 2/KI solution (I 2 = 2.5 x10 mol sharp exothermic peak is ascribed to the oxidation L-1 and KI = 6.5 x 10 -3 mol L -1 ) and then adjusted of the organic matter. The profiles of the TG and to a final volume of 50 ml. The contents were DTA curves in this step, suggest that the oxidation allowed to stand for 15 min at ambient tempera - of the organic matter is accompanied by combus - ture, before absorbance measurements at 600 nm. tion. The last step, between 365 – 520 oC, with loss of 23.6 %, the mass loss occurs through a slow process corresponding to the small and Results and Discussion broad exotherm between 370 and 410 oC and a sharp exothermic peak at 509 oC is attributed to The simultaneous TG and DTA curves of the total oxidation of the organic matter. the European chestnut and Paraná pine seeds The TG-DTA curves of Paraná pine seeds (pinhão) starches are shown in Figure 1. starch, Fig 1(b) show mass losses in three con - secutive steps, in spite of the second mass loss to suggest two overlapping steps, and thermal events corresponding to these losses. The first mass loss observed between 30 – 128 oC, with loss of 9.4 %, corresponding to the endothermic peak at 104 oC is attributed to the dehydration that occurs in a single step. The anhydrous compound is stable up to 276 oC and above this temperature the thermal decomposition occurs in two consecutive steps between 276 and 550 oC. The first mass loss observed between 276 and 386 oC with loss of 70.5 %, corresponding to the endothermic peak at 310 oC, followed by a sharp exothermic one at 342 Figure 1. Simultaneous TG and DTA curves of: (a) oC is attributed to the thermal decomposition that European chestnut seeds starch, m = 9.46 mg, and initiate without oxidative process, followed by (b) Paraná pine seeds starch, m = 8.62 mg. oxidative one. The second mass loss that occurs between 386 and 550 oC, through a slow process with loss of 20.1 %, corresponding to the exother - The TG-DTA curves of European chestnut mic peaks at 381 and 538 oC, respectively is attrib - starch seeds, Fig 1(a), show mass losses in four uted to total oxidation of the organic matter.
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