Made available in DSpace on 2017-07-21T18:53:17Z (GMT). No. of bitstreams: 1 FERTONANIH.pdf: 1031901 bytes, checksum: 493503a6add273da1bf51a7eec7dd483 (MD5) Previous issue date: 2006-08-17 / words: pectin, apple Apple juice processing may produce around 20-40% of the raw material as a by-product known as pomace, which could be useful as natural source of many high value compounds. The objective of this work was to establish a procedure of acid extraction of pectin from such industrial by-product. Aplle pomace, obtained in laboratory scale, was dried to decrease its chemical and microbiological instability. With essays at 97o C/10min seven acids were tested (1-750mM) in what concerns their effects on pectin yield and best acid was identified. Pectin was extracted according to a experimental design factorial 22 axial with repetitions at the central essay considering the effects of HNO3 concentration and time. The resulting model was analysed in what concerns regression and lack of fit. The pectin fraction obtained at the central essay was compared to commercial samples of low and high methoxyl pectin with titrimetry and spectroscopic FTIR techniques as well as by size exclusion chromatography and neutral sugar composition. The extraction reactions showed the difference of the nitric, hydrochloric, succinic and lactic acids, which an increasing yield up to 100mM from the trichloroacetic, malic and citric acids, with and increasing yield up to 750mM, reaching higher levels than possible. Nitric acid was the select and reaction containing 10 g of apple pomace gave better results than that with 5 or 25 although he yields were all the same (R2=). The model was statistically significant concerning gravimetric yield (R2 = 0.9834) and predicts that at 126mM and during 14 min it will be reached a maximum yield of 20.07 g/100 g. The same experiment established the model statistically significant (R2=0.9888) which predicts the minimum degree of esterification of 43,73% in extracted pectin at 200 mM during 10 min. The experimental sample of pectin (10 min, 100mM, 97° C) was similar to the commercial low methoxyl pectin both by titrimetric techniques as well as spectroscopic FTIR, and showed a similar HPSEC profile and ramnose insertion frequency in main acid chain. The results suggest the utilization of the model in conditions even milder than that of the central essay for obtaining low methoxyl pectin with less possibility of structural damage. Kepomace, yield, degree of esterification. / O processamento de suco concentrado de maça pode acarretar a disponibilidade de 20 a 40% da matéria-prima sob a forma de resíduo agroindustrial, o bagaço, que pode ser usado como matéria-prima para a obtenção de compostos de alto valor. O objetivo deste trabalho foi estabelecer um procedimento de extração ácida de pectina a partir do bagaço da maçã. O bagaço foi obtido em nível de laboratório e desidratado em estufa. Foram feitos ensaios com 7 ácidos em diferentes concentrações de 1 a 750 mM, temperatura de 97ºC por 10 min, para verificar o efeito sobre a reação da extração. Com o ácido mais adequado, foi utilizado um planejamento fatorial 22 axial com repetições no ponto central para estabelecer o efeito da sua concentração e do tempo, a 97oC, sobre o rendimento e a esterificação da pectina. Os modelos foram analisados estatisticamente com relação à regressão e a falta de ajuste. A fração de pectina obtida no ensaio central do experimento foi comparada com amostras comerciais de pectina de alto e baixo grau de esterificação em termos titulométricos, espectroscópicos (FT-IR), cromatografia de exclusão em gel e em relação ao seu conteúdo de açúcares neutros por cromatografia gasosa. As reações de extração evidenciaram a diferença entre os ácidos nítrico, clorídrico, succínico e lático, com rendimento crescente ate 100mM, e os ácidos tricloroacético, málico e cítrico, com rendimento crescente até 750mM chegando a valores superiores aos teores existentes de pictina. O ácido nítrico foi o que apresentou resultados mais coerentes e a reação de extração com 10 g de bagaço de maçã apresentou maior praticidade em comparação com 5g ou 25g embora os rendimentos tenham sido todos iguais (R2 = 0,9978). O modelo de extração ácida de pectina foi estatisticamente significativo (R2 = 0,9834) e demonstra que a 126mM durante 14 min dever haver um rendimento máximo de 20,07 g. O mesmo experimento definiu o modelo estatisticamente significativo (R2 = 0,9796) que demonstrou o grau de esterificação mínimo de 43,73% de pectinias extraídas a 200 mM durante 10 min. A amostra de pectina experimental (10 min, 100mM, 97º C) foi similar à comercial de baixo grau de esterificação tanto por titulometria quanto por espectroscopia FTIR, apresentou semelhante perfil de exclusão estérica e grau de inserção de ramnose na cadeia principal. Os resultados sugerem o uso do modelo em condições ainda mais brandas que as do ensaio central para a obtenção de pectinas de baixo grau de esterificação com menores possibilidades de danos estruturais.

Three dimensional printing (3DP) is one of the most important solid freeform fabrication (SFF) methods that can produce any material with desired 3D shape by using suitable powder-binder formulations. It differs from the standard molding operations in that it can produce a complicated shapes by a software driven instrument in a laminated fashion and the cost is lower. This method can be applied in a very wide area including drug release operations, biomaterial production especially for bone fixation, prototype production for all purposes, wound dressing etc. It can also be used in obtaining edible objects by using natural polysaccharides with water based binders. In this study, it is aimed to understand the gelling behaviour of some of the gelling materials, which are alginates, pectins and carageenans, and effect of various factors on the production of confectionary objects by means of 3DP process. Effect of multivalent cations, especially Ca2+ ion, on the gelling behaviour of these materials are investigated. The egg-box structure obtained between the polymer segments increases the water holding capacity of the materials and much more chewy structures can be obtained. The molecular changes are followed by Fourier Transform infrared spectroscopy (FTIR). In 3DP applications, the composition of powder and binder, pH, temperature, relative humidity (RH) and machine parameters are important factors affecting the texture of the final object. The texture of the produced specimens is examined by using a texture analyzer and maximum force values are given as g/cm at failure. Alginate and carrageenans are found to be more effective in obtaining chewy textures with Ca2+ ion content in sugar based matrices and optimization of machine parameters are performed to obtain a higher resolution on the specimens.