Central Food Research Institute 2008.

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1 Ph.D. Thesis ANIKÓ MATUSEK APPLICATION OF FRUCTO-OLIGOSACCHARIDES IN OSMOTIC DEHYDRATION BY DIFFUSION AND DEGRADATION KINETIC APPROACH Supervisor: Consultant: Dr. Bálint Czuor Dr. Feren Örsi Central Food Researh Institute 008.

2 1. INTRODUCTION, AIMS The guiding priniples of the modern nutrition enourage the food produers and food sientists of the 1st entury to develop new, healthprotetive funtional food produts, whih maintain the human health, an be applied in up-to-date diets and are attrative for the onsumers. With full nowledge of the domesti nutrition habits, it is important, that the fruit and fiber onsumption of the Hungarian population is very small. The fiber enrihed foods lie fruit produts enrihed b y frutooligosaharides are of overriding importane in the field of funtional food development. Fruto-oligosaharides have several nutritional benefits; prebioti ativity ould be the onsiderable of them. Osmoti dehydration fits well into the tehnology of dried fruit produts, whih eliminate the seasonal nature of fruit onsumption beside their evident values. Osmoti dehydration is a water removal proess. Due to the transport phenomena espeially solid gain in the tissues - ourring during this tehnologial unit operation funtional omponents ould be introdue into plant matrix. Fruto-oligosaharides are not yet nown as osmoti medium based on the available sientifi literature. Due to their nutritional benefits, they ould be funtional food omponents. The enrihment of fruit matrix with frutooligosaharides by diffusion ame forward as a real industrial problem, whih has to be solved therefore, I set to my study the aim to investigate the tehnologial appliability of fruto-oligosaharides as osmoti agent. The aims of the study: Comparative investigation of the diffusion oeffiient of frutooligosaharides (Raftilose P9, ORAFTI) and surose, srutinizing the unique diffusion oeffiient of eah oligomer omponent, desribing the transport phenomena.

3 Investigation of the effet of treatments arried out before osmoti deh ydration (blanhing, mirowave-treatment) on the texture, ellmembrane permeability, hanges of the solid ontent, additionally on the transport phenomena ourring during osmoti dehydration in apple model (Malus domestius v. Idared). Charaterization of the osmoti deh ydration ombined with vauumtreatment, investigation its effet on the dehydration quality and fruit texture. Determination the rate of hydrolyti degradation ourring during tehnologial unit operations. Kineti study of the degradation based on laboratory simulation.

4 . EXPERIMENTAL AND CALCULATION METHODS Determination of arbohydrate omposition by HPLC (Mer & Hitahi system, L-00 pump; Waters 0 differential refratometer; D 00 Integrator; Spherisorb SQ NH (SUPELCO) olumn, aetonitrile-water eluent. Measurement of tissue permeability (Labvig ondutometer with 100 ell). Determination of the texture properties (Lloyd LR-K texture analyser Nexygen software; SMS TA.XT. Plus texture analyser Texture Exponent software. Dry matter and water ontent determination by gravimetri method; determination of soluble solid ontent (Carl Zeiss refratometer); volume measurement by granula exlusion, determination of density and porosity (pinometer 1/99). Sensory evaluation by soring. Charaterization of the water loss (1) and the solid gain (); determination of the diffusion oeffiient (): mb ( MCb /100) mod ( MCOD /100) WL = (1) m ( TSC /100) b b mod ( TSCOD /100) mb ( TSCb /100) SG = () m ( TSC /100) b b D eff m a = () Fo (1)-(): WL: water loss, g/g; SG: solid gain, g/g; m: mass, g; MC: moisture ontent, w/w%; TSC: total solid ontent, w/w% (b: after blanhing; OD: after osmoti dehydration) (): D e f f : effetive diffusion oeffiient, m /s; m: slope of the funtion: ln 0 - f(t), Fo: Fourier number

5 Kineti desription of fruto-oligosaharide degradation by numeri solving of ()-(10) differential equations (Maple 9 - Maplesoft ). dt d = () dt d = () dt d = () dt d = () dt d = (8) 1 dt d = (9) 1 1 dt d = (10) ()-(10): i : i onentration of oligomer having degree of polymerization: i; j i : rate onstant of the degradation of oligomer having degree of polymerization i to oligomer having degree of polymerization j Statistial evaluation was arried out by Exel (Mirosoft) and Statistia.1 softwares (StatSoft).

6 . NEW SCIENTIFIC OUTCOMES I. I have proved that the input of fruto-oligosaharides into apple tissue by diffusion has aeptable rate from tehnologial aspet. Based on this fat there is possibilit y to develop funtional (e.g. prebioti) frutooligosaharide enrihed fruit produts by applying osmoti dehydration. /Matuse et al. (00) Élelm Ipar LIX(1), 18-0.; Czuor et al. (00) Konzervújság,, 9-9.; Matuse et al. (008) Innov Food Si Emerg Tehnol, in press/ There is not any differene between the physial properties of the samples - treated by the two different osmoti media - after blanhing. However, after osmoti dehydration signifiant alteration was observed in their texture. The elastiity oeffiient inreases, the hardness of the fruit does not alter during osmoti dehydration in surose solution, meanwhile both of the two physial parameters deline by 0-0%. II. I have established that the diffusion rate of fruto-oligosaharides and surose are in the same order. The diffusion of fruto-oligosaharides is more hindered than that of surose; it is a signifiant differene in the deh ydration apaity of them. The deh ydration apait y of frutooligosaharides is less at room temperature, but it inreases by the temperature, and it is better than for surose at 0-0 C. /Matuse & Merész (00) Per Pol, (1-), 8-9.; Matuse et al. (00) Hung J Ind Chem, (1-), -8.; Matuse et al. (00) Élelm Ipar LV III(), ; Matuse et al. (008) Innov Food Si Emerg Tehnol, in press/ The surose gain is just twofold higher than the fruto-oligosaharide gain however, the value of water loss is only by 0-0% greater. In ase of osmoti dehydration by surose tissues have higher onentration of sugar regarding to the higher amount of soluble solid flowing into them whereas in ase of fruto-oligosaharide solution, the water loss auses same refration in the tissues. The refration of the tissues being the resultant of the two transport phenomena does not alter signifiantly in ase of the two osmoti media.

7 III. I have found that the unique diffusion oeffiient of oligomer omponents do not alter signifiantly from eah other. The effetive diffusion oeffiient of dimer is 0, sine steady state exists related to it. /Matuse et al. (008) Eur Food Res Tehnol, in press/ The amount of monomer moleules derease by the time of osmoti dehydration, sine the onentration of them in the untreated fruit is higher, than in the oligomer mixture ontaining only a little amount of monomer. Hene, it diffuses from the fruit tissues into the solution. The amount of dimer moleules (mostly surose) is onstant in the investigated range of the treatment. The amount of oligomers having higher degree of polymerization (DP-DP) inreases logarithmially in the funtion of diffusion time. The values of effetive diffusion oeffiients are,-, 10-9 m/s. Based on the assay of transport phenomena neither the surose nor the fruto-oligosaharide gain are not affeted by the temperature and time of blanhing. On the ontrary, water loss is influened by these tehnologial parameters. Water loss inreases by the inrease in the temperature and time of blanhing. The hanges are stronger in ase of surose. Heat treatment auses signifiantly lower hardness omparing to the untreated sample. The inrease of heat treatment temperature from 0 C to 0 C deline the value of hardness signifiantly, while further inrease by 10 C does not hange the hardness signifiantly. The elastiity oeffiient derease signifiantly under the treatments omparing to the untreated sample, but the other blanhing parameters do not alter its amount signifiantly in the studied range. Blanhing auses derease in the mass of the apple samples due to the damage of tissue struture, this is stronger in ase of oligofrutose solution. Fruto-oligosaharides soften more the struture of the fruit. It is an important alteration between the two blanhing agent, that after the pre-treatment by oligofrutose followed by osmoti dehydration the mass loss is by -% higher (18-0% ompared to 1-1%).

8 In ase of mirowave treatment, the derease of hardness is more notable than in ase of onventional blanhing. The mirowave treatment time and temperature have signifiant effet on the elastiity oeffiient and hardness. The tissue permeability inreases monotonous by the inrease of blanhing temperature. The inrease of temperature to 0 C the effetive diffusion oeffiient inreases (, 10-9 m/s), the alteration on higher temperature is not signifiant. The tissue permeability inrease monotonous and signifiant also affeted by mirowave treatment. The value of diffusion oeffiient inreases signifiant by the temperature. IV. I have showed that the vauum-treatment does not alter the diffusion rate during osmoti dehydration operation. I have established that the tehnologial advantage of the ombined vauum-blanhing pretreatment is the inrease of tissue permeability, but its drawba is the damage of the texture properties. /Matuse et al. (008) Eur Food Res Tehnol, in press/ I [µa] ontroll 0 C 0 C 0 C 80 C t [per] 1,8 1, 1, 1, 1,0 0,8 0, 0, 0, 0,0 Fig. 1. Change of tissue permeability, ion-diffusion oeffiient in the funtion of vauum-blanhing temperature Deff10 9 [m s -1 ] ontroll 0 C 0 C 0 C 80 C T b [ C] During osmoti dehydration whih follows either onventional blanhing or vauum pretreatment similar diffusion oeffiient was observed: m /s. In the ourse of ombined pretreatment the tissue permeability inreases by the inrease of temperature (Fig. 1). The diffusion oeffiient inreases monotonous by the inrease of temperature, and was higher also in ase of treatment at 0 C. Between 0-80 C it inreased from to m /s. However, 8

9 the damage of texture properties emerges in the derease to one third of elastiity oeffiient, hardness and mass loss. V. I have proved that the degradation of fruto-oligosaharides is a protonatalyti proess and under tehnologially real onditions (ph=.-.) a hange by 0. unit in ph auses four fold alteration in the degradation rate. I have found that in buffered solution the ativation energy is 0-10 J/mol dependent on ph. /Matuse et al. (008) Ata Aliment, aepted; Matuse et al. (008) submit. Eur Food Res Tehnol/ [1/per] 0,0 0,00 1 0,01 0,010 0,00 0,000,,,8,9,1 ph Fig.. Degradation oeffiient in the funtion of ph at 80 C, in buffered solution The degradation of oligomers an tae plae under the onditions of proessing tehnologies (Fig. ), if ph is under. and the temperature exeeds the 0 C. By lower ph than.0 the apple matrix, namely the omponent of the apple aelerate the degradation proess (Fig. ). Several theories an be drafted on the matrix effet of apple. First, the rate of degradation is atalyzed by the H onentration, moreover the aid omponent of apple an also aelerate, atalyze the proesses. 9

10 (1/per) 0,0 0,0 Puffer-pH, Alma-pH, Puffer-pH,0 Alma-pH,0 Puffer-pH, Alma-pH, 0,0 0,0 0,0 0,01 0,00 1 Fig.. Degradation oeffiients in the funtion of number of oligomer units at different ph (.-.0-.) in buffered solution and apple pulp VI. I have showed that the rate of degradation depends on the degree of polymerization. Aording to the ativation energy, the degradation rate of oligomers having higher degree of polymerization (DP-) is signifiantly greater. /Matuse et al. (008) Ata Aliment, aepted; Matuse et al. (008) submit. Eur Food Res Tehnol/ E a (J/mol) ph, ph,0 ph, Fig.. The ativation energy alulated by the summarized degradation oeffiient in buffered solution (-, -, -, -, -, -: sign of the number of oligomer units) 10

11 VII. I have proved that among the possible degradation paths the rate of reation that auses end-hain degradation is higher than the rate of inside-hain hydrolysis. /Matuse et al. (008) Ata Aliment, aepted; Matuse et al. (008) submit. Eur Food Res Tehnol/ Table 1. Degradation oeffiients aording to degradation paths (80 C, ph=.; buffered solution) Degradation oeffiient (1/min) End-hain degr. Inside-hain degradation 0,0 0,00 0,00 0,018 0,00 0,00 0,018 0,00 0,01 0,00 0,00 1 0,00 Fig.. Comparison of the alulated and measured oligomer and monomer onentration (Degradation of tetramer and formation of monomer (80 C, ph=.; buffered solution) 11

12 . APPLICATION The input of fruto-oligosaharides into apple tissue by diffusion has aeptable unit operation rate. Based on this fat it is possible to develop funtional (e.g. prebioti) fruit produts, whih are enrihed b y frutooligosaharides by applying osmoti dehydration. The results of tehnologial and ineti experiments summarized in the Ph.D. thesis an be utilized in the development of foods enrihed b y frutooligosaharides. The adapted methods help the tehnologial planning and are suitable for the investigation of the produts. Several types of prodution tehnologies an ontain the step of osmoti dehydration, as the method to enrih tissues in funtional omponents, so exat tehnologial reommendation ould be suggested only in view of the end produt. However, some general guide-lines ould be stated: In the proessing tehnology of fruits applying fruto-oligosaharides under the natural ph (.0) the operation temperature should not exeed the 0 C, avoiding the degradation of fruto-oligosaharides. For an apple based produt having high value and good organolepti properties, blanhing of the raw material in isotoni solution and osmoti dehydration at low temperature (<0 C) ould be suggested. The osmoti dehydration ombined by vauum-treatment ould be used by suh a speial produt group, semi-final produts, when the damage in the texture properties is not important beause of the further tehnologial proessing resulting a more omplex food matrix, where the osmotially dehydrated material is only a omponent of the end produt. 1

13 . PUBLICATIONS RELATED TO Ph.D. THESIS Papers in English 1. Matuse, A., Merész, P. (00). Modelling of sugar transfer during osmoti dehydration of arrots. Periodia Polytehnia Ser. Chem. Eng., (1-), Matuse, A., Czuor, B., Merész, P., Örsi F. (00). Mathematial modelling in osmoti dehydration. Hungarian Journal of Industrial Chemistry, Speial Issue on Reent Advanes in Computer Aided Proess Engineering, (1-), -8.. Matuse A., Czuor, B., Merész P. Comparison of diffusion of fruto-oligosaharide omponents during vauum impregnation and osmoti dehydration, European Food Researh and Tehnology, In press, Available online: 00. augusztus. IF: 1,08. Matuse, A., Czuor, B., Merész, P. Comparison of surose and frutooligosaharides as osmoti agents in apple. Innovative Food Siene and Emerging Tehnologies, In press, Available online: 00. november. IF: publishing in Matuse, A., Merész, P., Le T. K. D., Örsi F. (008) Fruto-oligosaharide degradation in apple pulp matrix, Ata Alimentaria, In press IF: 0,. Matuse, A., Merész, P., Le T. K. D., Örsi F. (008) Effet of temperature and ph on the degradation of fruto-oligosaharides, Submitted to European Food Researh and Tehnology IF: 1,08 Papers in Hungarian:. Matuse, A., Czuor, B. (00). Fruto-oligoszaharido felhasználási lehetıségei gyümölsészítményeben. Élelmezési Ipar, LIX. (1), Czuor, B., Matuse, A., Léder Ferenné., Shusterné Gajzágó, I., Vásárhelyiné Perédi, K. (00). Az egészségmegırzést szolgáló minıségnövelı anyago alalmazása élelmiszere elıállításánál. Konzervújság,., Matuse, A., Czuor, B., Merész, P., Örsi F. (00). Szaharóz és frutooligoszaharido diffuzivitásána összehasonlító vizsgálata almán. Élelmezési Ipar, LVIII. (), Matuse, A., Czuor, B., Merész, P. (00). Az ozmotius dehidratáió élelmiszeripari alalmazásána szempontjai és modern megoldásai. Élelmezési Ipar, LVII. (),

14 Proeeding in Hungarian: 11. Matuse, A., Czuor, B. (00). Az ozmotius dehidratálás mővelete a gyümölsfeldolgozás folyamatában. Mőszai Kémiai Napo 0, Veszprém, 00. április -8., Konferenia Kiadvány, -. Summary in Hungarian 1. Czuor, B., Matuse, A., Léder Ferenné., Shusterné Gajzágó, I., Vásárhelyiné Perédi, K. (00). Minıség növelést élzó anyago alalmazása élelmiszere elıállításánál. Konzervújság,.,. Poster presentations in English: 1. Matuse, A., Czuor, B., Merész, P. Fruto-oligosaharides in the funtional food development. The First International Congress on Food Safety (SAFE Congress), Budapest, June, Matuse, A., Czuor, B., Merész, P., Örsi, F., Kupezi, M. Comparative investigation of the osmoti behaviour of surose and fruto-oligosaharides in apple. th International Conferene on Food Siene, Szeged, 0-1. May, Matuse, A., Czuor, B., Merész, P., Örsi, F. Osmoti enrihment of apple by frutooligosaharides. nd Central European Food Congress ( nd CEFood Congress), Budapest, -. April, 00. Poster presentations in Hungarian: 1. Matuse, A., Léder Ferenné, Czuor, B. Kedvezı érzészervi tulajdonságú prebiotius fruto-oligoszaharidoal dúsított élelmiszere. Magyar Táplálozástudományi Társaság XXXI. Vándorgyőlése, Keszthely, -. Otober Czuor, B., Matuse, A., Merész, P., Örsi, F. Diszaharid és oligoszaharid ozmózisos hajlamána összehasonlító vizsgálata almában. Lippay János Ormos Imre Vas Károly Tudományos Üléssza, Budapest, -. November 00. Leture in English: 18. Matuse, A., Czuor, B., Merész, P., Örsi, F. Mathematial modelling in osmoti dehydration. 10 th International Worshop on Chemial Engineering Mathematis, Budapest, August 00. 1

15 Letures in Hungarian: 19. Matuse, A., Czuor, B., Merész, P., Albó, N. Váuum-ezeléssel ombinált ozmotius dehidratálás vizsgálata almán. Lippay János Ormos Imre Vas Károly Tudományos Üléssza, Budapest, Otober Matuse, A., Czuor, B. Prebiotius szénhidráto felhasználása gyümölsészítményeben.. Országos Mezıgazdasági és Élelmiszeripari Kiállítás (OMÉK), Fiatal Kutató Fóruma, Budapest, 1 September Czuor, B., Matuse, A., Léder Ferenné., Shusterné Gajzágó, I., Vásárhelyiné Perédi, K. (00). Minıség növelést élzó anyago alalmazása élelmiszere elıállításánál. XXXVII. Nagyırösi Konzervipari Napo Tudományos Tanásozás, Nagyırös, May 00.. Matuse, A., Czuor, B. (00). Az ozmotius dehidratálás mővelete a gyümölsfeldolgozás folyamatában. Mőszai Kémiai Napo 0, Veszprém, 00. április -8., Konferenia Kiadvány, -.. Matuse, A., Czuor, B., Örsi, F. Az ozmotius dehidratálás vizsgálata almán. II. Dotoráns Konferenia, BME,. November 00.. Matuse, A., Czuor, B. Gyümölsészítménye elıállítási tehnológiájána idolgozása fruto-oligoszaharidoal. A Magyar Táplálozástudományi Társaság XXIX. Vándorgyőlése, Hajdúszoboszló, 8-0 Otober 00. 1

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