LWT Food Selence and Technology 141 (2021) 110851 Contents lists available at ScienceDirect ie LWT journal homepage: vw. elseviercomilocatliwt Dry-heat treatment vs. heat-moisture treatment assisted by microwave eae radiation: Techno-functional and rheological modifications of rice flour Angela Garcia Solaesa’, Marina Villanueva", José Maria Munoz’, Felicidad Ronda” * Dement Agence ond ery Experi Fod Tess, PROCERELich Recah Crap. Cale of alr on For geri Unies of ats, sa Deron of Eucoty and Bevo Ur of Ya, Yala pan ARTICLE INFO AnsTRACT ee four Pes properties ‘at elo! popes “The eapacy of microwave (MW)assied dey eat and beatmolute wesiments wo madly wchno functional Doperties and gel viscolastly of rice Aout was studied Flour samples at 30%, 209% 19%, 13%, a, and Ss of metre content (HC) vere microwaved fr 440s at Wg, The 3% MC sample was unmodified by ‘wean However, dhe 8¥ MC saple was one of the most fected, along with the 20% and 30% samples, Indicating that asl amount of water can plstiie tee our enough to eatange its bopayers mleeaks (awaily stare) respensibe forthe medications. The lowest peak and breakown viscosities andthe highest pasting temperature were found in te 30% MC sample, which varied ~58%, ~80%, and +8 °C respectively, from native four, DSC reveled partial pe geatinizacon in the 2086 and 09% MC samples. Sweling power increse in all apes ner eaten, whe water soit only incensed in the Bnd 30% MC samples ‘Treatments promoted gel stability and enianeed viscoelastic mod, pariclavy inthe 8% and 20% MC am Pes Flour MCin MW assisted reat allowed the radaltion of eho factional properties frie Nou and TBecloicl wd thernd carecteias of he gs, 1. Introduction ‘w/w and high temperatures (2110 °C) for 14h (Ku, B90, Chen, & ‘Gao, 2010) tis assumed that in both HMT and DHT the structure of the Research efforts in the manufseture of gluten-free (GF) products starch granules is not destroyed (Srayovean Nena, 2014. have rapidly increased over the last decade. Various spprosches are being used to improve the quality of these products, which general Ihave poor sensory propertes. Physieal methods such as heat noistre trentments and annealing appear to be good alternatives to improve aluten free dough and bread characteristis (Villanueva, Harasyn, ‘uiloz, & Ronda, 2019). They are considered to be safer and more ‘environmentally friendly compared to chemical modification (Oyeyinka, Umaru, Olatunde, & Joseph, 2019), Heat moisture treatment (HMT) is by far the most studied method of physical modification of starch. Typically, HMT utilizes high moisture contents (20-358) and temperatures (>90 °C) for long treatment pe ods (1-24 h). However, dry-heat treatment (DHT) has recently received a great deal of atention because of its simplicity and safety. DHT isa physial modification thar can affect the starch grams t0-8 ‘erin extent and change the structure ofthe erystelline and amorphous regions of starch and, as a consequence, is physicochemical properties. “The usual DIT conditions include the use of low moisture levels (<103% Fal ees fina. (Rnd np//dotng/101016/. 5. 2021.110861 Rice (Oryza sativa.) one ofthe most important cereal crops inthe ‘world. In addition to whole rice, global rice flour production has Increased significantly dve to its hypoallergenic proteins and Tack of| -luren, which make i essential i the formulation of GE products (Wl Tne, Harasymi, Muon, & Ronda, 2018), Many works have studied the physical modification of rice four by HMT (moisture content of 20-258) (Pnchn-arnon & Utiapap, 2019), Recently, the effects of DHT ‘on the structure and physicochemical properties of rice starch have also ‘been investigated (jung, Young, & Gy, 2018) The effet of both treatments, HM and DHT, depends on several variables such as type of| starch, moisture content (MC), temperature, and time of heating Geniller, 20185 Bragoveanu & Nemjanu, 2014), Almost universally, DIT decreases starch solubility, swelling power, amylose leaching, and peak viscosiy, and increases pasting temperature (Sisco, Rul, Sr ‘keeo,& Segovia de In Revilla, 2018). In the ease of DHT, It seems to Increase gel strength and pasting visesity above 130 °C, at short ‘westment periods, whereas both were reduced with Increasing heating Received September 2020 Received in eve form 26 December 2020; Accepted 30 December 2020 Available online 6 Janay 2021 (0023 6438/6 2021 Heer i All sights eeetime, Furthermore, the amylose content of ree starches influenced thelr pasting, physicochemical, and theological properties after DAT (King etal, 2018), ‘Traditional heating systems used in both HT and DH are often ‘expensive and difficalt 10 implement on a large seal; so alternative methods sch as microwave (MW) heating, have been investigated (Si, ‘Cotineeranat, Licks, & Chatakasonda, 2018), K provides fst, uniform heating, and it is economical and environmentally friendly, at mini ‘izes energy consumption (Su, Xo, & Xiong, 2014). Te has demon strated effects onthe structure and physicochemical properties of cereal, tuber, and legume starches (Srasovenn & Nemfanu, 2014). Several factors suc 8s MW time and power, MC, and botanical source of four may significantly influence the physleochemieal properties of the treated flour (oyevinka eal, 2019). Mast ofthe literature refers to MW heating of starches under HMT conditions, while very few studles applied DHT conditions, with water content <159%, eventhough I was shown that low moisture starch samples underwent transformation iferently from high moisture samples (Levicka, Siemon, & Kurcok, 2015), Most of the work found in literature used commercial MW ‘equipment, where dhe our was irradiated in non-hermetc containers Grasoveania & Noman, 2012, Aliough the evolution of the Now MC during treatment is generally not reported, it has been seen that iti ‘quickly lost overtime, reaching very ow values, lose to the mouo layer ‘water content ofthe flour, after some few minutes of treatment (V1 ‘mucva, Harasym, et al, 2018). Therefore, MW treatments are often tnised HMC-DH treatments that do not facilitate establishing the exact role of sample MC inthe changes experience, since I varies over tne In this study the rie flour MC was kept constant during MW radiation using a hermetic container and MCS ranging from 3% (feeze dried sample) 103096. The effect of MC: during MW treatment on the phys ‘ocheaieal and pasting properties of rice lour have been evaluated for the frst time ro establish the relative Importance of the plsteiing ef fect of water and the temperature reached by the four ding treatment in modifying these properties. The MC values tested ranged from 3% 10 ‘8% (very low/low vale that could be classified within DIT processes) to 20% and 30% thigh values, classified within the HMT processes) passing through 13% and 15% (natural MC of flour and intermedi value located in the border between DHT and HMT) The impact of treatment on the thermal and viscoelastic properties of gels made with Ilerowaved flours was also established, 2. Materials and methods 2a. Somes nia ice dong grain) flour was kindly provided by Herba Ricemills SLU. (Valencia, Spain). The MC was 13%, ash <0.9%, protein >6.58, fae <1%, and glaten <10 ppm. The Nour granlometty was: > 250 yam (4%), 210-250 ym (10-2096), 150-210 um (85-4596), 100-150 ym (20-358), and <100 ym (10-2086) (data provided by manufacturer. 22. Preparation of het treated rice flour Rice flour MC was mewsired with the AACC 4-19.01 Oficial Method (VAC, 1999). Six batches at diferent MCs of 39%, 89%, 13%, 158, 208, and 30% + 0.586 were prepared. The MC of 3% was obtained by rice flour lyophilization in PreeZone 1, Labcanco lyopilizer (Kansas ‘ity, USA). The MC of 9% was obtained by drying the native lou in an incubation chamber (Memmert ICP260, Schwabach, Germany) at 40 °C until the desired MC was achieved. The natural rice four MC was 13%. ‘The water needed to reach the levels of 159,208, and 30M was added as was described by Villanueva, Hatasym, etal. 2018). 2.3. Microwave mearment ‘A000 W sharp MW oven (REA2INW) (Sakai, Japan) was used 10 wr 41 aon 130851 perform the MW treatments. 50 g of Nour at desied MC levels were exposed to MW radiation (100% power) for 480 sin eyeles of 10 ra lation and 60 sof rest in hermetic Teflon® container (volume of 1000 sn}, twas constantly sired during treatment xs was described prev ‘ously (Vllaneva,Havesyn, et al, 2018). The temperature reached i cael treatment was measured by Testotem® temperature strips fon "TESTO (Barcelona, Spain), which were placed inthe container in per ‘manent contact with the flour sample following the procedure described by Villanueva, Harasym, etal (2018). After cooling to room tempera ture, the samples were sieved to <250 um for further analysis. The MC of| the samples was checked after treatment and it was verified thet the MC did not change more than 0.6 fron its initial vale, Samples at 206 and 50% MC were dried at 5 °C until getting back 10 13% t0 avoid spollage. Untreated rice flour was used as contol. Each treatment was carried out in triplicate 2.4. Apparent anpose convent Apparent amylose content (AAC) of native and microwaved flours ‘was determined wsinga K AMYL assay kit (Megezyme Intemational Ld Ireland), The absorbance was read at SLO nm. Three replicates were rade for each sample, 25. Hydration properis ‘Water absorption capacity (WAC), water absorption index (WALD, ‘water solubility index (WSD, and swelling power (SP) of rice flour simples were mensured, Two grans ofeach sample were mixed with 20, ‘mL of distilled water in 50 mL centrifuge tubes. WAC ( water retained {flour dry matter (din) was determined following see, Colla, sue onda (2015). WAL WSL, and SP of the flours were caleulated as Aeseribed by Abebe etal. (2025), with slight modifications. The dis. persions were cooked for 15 min at 95°C, cooled 10 room temperate, and centrifuged at $000%g for 10 min. The supernatant was poured into 4 pre-weighed evaporating dish to determine its soluble solids content, and the sediment was weighed (WAL, g of sediment/g flour dm). The ‘eight of soluble solids by evaporating the supematant overnight at 110°C (WSI,gof soluble solids /100 g lou dm) and SP (g of sediment/g Insoluble solids Nour dim) were calculated 26. Color characteris Color measurements of ree four samples were carted out using & PE Instruments colorimeter (PCE GSMS) in CIELAB coordinates with 10” standard observer and D6S standard illuminant; L* indicates light ness, a* varies from green (~) to ed (4) and b* from blue (10 yellow (C1). The he (H) and the eliroma (G°} were also obtained from the CCHELAB coordinates. Color difference (AE) ofeach treated sample with respect to control wes calculated with the esation: AB = (aL? + (aah + (aDeyy!® ach sample was measured five times. 2.7. Pasting properties Pasting properties of starch were determined with a Kinexus Pro + ‘heometer (Malvern tnsteumeats, 11K) equipped with a starch cell Each ree flour sample (3:5 14% moisture basis) was mixed with 25 ¢ of distilled water before loading into the starch cell. Paddle speed was 160, ‘pm during the test. The sample was heated following the method described by Villanova, Harasym, otal. 2018). The pasting tempera ture (PT, peak viscosity (PV), trough viscosity (TV), breakdown vs cosity (BV), final viseosity (FV), and setback viscosity (SV) were recorded, The determination was carried out in duplicate.2.8. Rheolgical properties of gels nude from microwaved rice flours ‘The theological ests were carried out 15 min after preparing the gels ollowing the protocol described in Section 2.7) to allow sample relaxation. Strain sweeps were carried ut rom 0.1 10100086 strain at Hz frequency. From these curves, the maximum stress na) beyond Which the dough structure was broken (corresponding 19 the linear viscoelastic zone, LVR) and the stress atthe eross point (G" = G") were ‘established. Frequency sweeps were carried out from 1 to 10 Hz inthe linear viscoelastic region (LVR); the stn value chosen for the fe {quency sweep tests ofall gels was 1%, which was within the LVR. The frequency sweep data were fitted to power law model (Villanuevs, De amo, Harasym, © Ronda, 2018), The values G'y and G", and (tan 8) fare the coefficients obtained front the fitting to the power law and Tepresent the elastc and viscous modull and the loss tangent, espec: Lively, ata frequency of 1 Ha. The a band values are the exponents of the ited potential equations ad quantify the dependence ofthe elastic and viseous moduli and the loss tangent on the oseillaton frequency. Bach test was carried out in duplicate, 2.9. Gelatnzation ad retrogradation properties ‘The watreated snd the microwaved-rice Aours (~6 me) with an ‘excess of water (70% water) were weighed in 440 wLaluminu pan and heated from 0 t0 115 °C at 5 “C/min in a Differential Seanning Calo ‘meter (DSC3, STARE System, Meter Toledo, Switeerland) using an ‘empty sealed pan as reference, The gelatinized samples were kept inthe pans at4 4 2"C and after 7 days they were measured again with the same method to smidy their retrogradation transition. The enthalpy of {gelatnization and retrogredation were recorded and expressed in J/g ‘ry matter (dm). The degre of retrogradation, DR (8), was established ‘as the enthalpy of rettogradaion divided by the enthalpy of gelatin zation. All messurements were petformes in duplicate 2.10, Statistical nays Statstenl analyses were conducted using the software Stargraphies centurion XVILX64 software (Bisiream, Cambridge, MN, USA). To check the statistleal importance of observed variability, one-way ANOVA was applied and the least significant dllference (LSD) at p. value <0.05 was used to separate meas, 15 16s as 135, vos 85 Flour Temperature °C) 65 4s 25 0 [28 wr 41 aon 130851 3. Results and discussion 3.1. Tenperanre and moisture evolution in flour during AW eearnent During MW processing the flour temperature vs. time profiles were significantly affected by MC (se Pix. 1). The hermetic Teflon® container used in this study made it possible to keep sample MC constant ‘throughout treatment. This fact had a significant impact on temperature profile. As can be seen in Fig. 1, flour temperature increased over ime ‘uni it reached, i 3-4 ain, a maximum vale that remained constant ‘uni the end ofthe treatment. Hoth the rate of temperature increase ad the maximum temperature reeched depended on the MC of the our ‘he final long plates of constant temperature corresponded ta period Inwhich the heat absorbed by the sample was equal the feat lost by it towards the container and from Ie to the surroundings (Villanieva, Hees, eta, 2018). The plateau temperarutes vaeied with the Nour MCs follows: 99-1 °C (88), 178 £4 °C (8H), 198 1 °C (19%), 141 29°C (15%), 186 43 °C (20%), and 114 + 3 °C (30%). The rate ofthe Temperature inerease during the first MW treatment segment vas ‘determined by two simultaneous processes governed by two properties ‘opendent on flour MC: STW absorption capacity and specific heat. The first property determines the flour'seapacity to transform MW radiation {nto heat, while the second one controls the amount of heat the flour needs to change its temperature. Both properties inrease with MC and hhave an opposite effect to the rising temperature profile (Villanova, assy, eta, 2018). Considering how these slopes evolve with four IMG, it seems that specific heat predominated in this step. The second ‘treatment segment (constant temperature) was controlled by the bal ance between the absorbed and the dissipated power. The heat transfer coefficient whieh inereases dramatically with the Mout MC and in parcieulae with the presence of saturated water vapor around the sa ple- explains the higher power dissipated betwoen the flour and the ‘Teflon container and the lower temperature of the plateau reached by the stmples with higher MCs. It should be noted thatthe MW absorption ‘capacity ofthe lr increases with MC only logarithmically (lla Hoarasym, et al, 2018). “The sample with an MC of 9 rose to the lowest temperature due to its very low MW absorption capacity from is low humidity (below the ‘monolayer MC, which in ice Nour is 5-69%) (Abebe & Ronda, 2015). Nevertheless, the sample temperature increase to 99 °C demonstrates ‘that even this very low MC (3%), strongly bound to dry matter, was ‘capable of absorbing MW radialon. The sample with 8 MC was found oo eo 7 Treatment time (min) Fig. 1, volition of temperate ofthe Nour during the MW teament a 8% (0), 1816 (0, 20% (A) and 306 (CD of motte contentat the opposite end of dhe range. I¢ rose to dhe highest cemperatne ‘because ofits Tow MC (only slightly above the monolayer level} this prevented the vapor inside the Teflon® conraner from reaching sat ration, reducing the hent transfer between the four and the walls ofthe container. The very high sample-surroundings thermal resistance led to ‘an increase in the equiibrivnn temperature seithin the sample, despite the stil low MW power absorbed, 3.2. Apparent anylose content (AAC) ‘The control flour used in this study could be elasfied as interme dlinte amylose lu based omits AAG, which was 16.4 0.96 (St, 2018). The AAC ofthe samples treated at 8% and 3096 MC were 20.7 = (0.496 and 18.6 + 1.1%, respectively, significantly higher than the native counterpart (Table 1). These two samples were the result of the most, severe conditions (with the highest temperature or MC, respectively). ‘The inerease in AAC in DHT samples was previously reported and ‘explained by the degradation of long-amylose chains into. many short amylose ones during dry heating proces (el sl, 2020). MMT may eause the thermal degradation of amylopectin exterior linear chains. Those degraded chains might become amylose ke, responsible for inereasing AAC, The rupture of amylose and amylopectin in teractions in the amorphous regions of stach granules would also release amylose and lead to higher AC values (H. Li, Lv, Peng, Shan, & ‘Wang, 2015) Amplopeetin damage presumably leads to a reduction in the amylopectin fraction and, hence, 10 a slight increase in AAC (©yeyinks et, 2019). The AAG contents ofthe samples treated at 36, 1396, 15%, and 20% MC were not significanty diferent from native flour AAC. 3.2. Hydration properties WAG, WAL and WS! of control and microwaved rice lours are shown In 8g. 2: SP included in Tle 1. The sample teated at 33 MC dl not show any significant change in these properties with regard to native flout. As demonstrated above, the energy absorbed by this sample was limited. The WACS of samples treated nt 356, 6, and 139% MC were the ‘sme as that of the control Rou (21.3 g/g). However, WAC Ineteased in samples treated at 15% (138), 20% (+4696), and 30% MG C469), under IMT conditions. These results might be attributed to disrupted hydrogen bonds between the amorphous and crystalline regions and a slight expansion of dhe astorphous region, improving the hydrophilic tendency ofthe starch molecules during HAT but not in DHT. These changes seem to be favored by a higher sample MC during thermal treatment (H. Live al, 2015). WAI Eig.2) and SP (abe 1 inereased in wr 41 aon 130851 all reated samples (except $% MC). The highest inerease in WAI was ‘obtained forthe samples treated at 8%, 133, and 15% MC 9 g/g 6 7.8 g/ forthe contol. In samples treated at 20% and especially at 30% IMG, the increment was less marked. A partial pre-geatinizaton caused by the high MC nnd temperature could explain the lower get hydration capacity of samples treated at 2086 and 30K ME (lag & Mizoneasa, 2019), In addition, the short amylose chains produced by heat hydro lysis, which easily dissociate and diffuse out of the granules during swelling (Kyung et al, 2018), would decrease sediment weight. WSI ‘increased significantly only in samples treated at 8% and 30% MC, fon (05% (contol Nou) to 2.63 and 2.91%, respectively, The increase i solubility may be a consequence of shrinkage and/or disintegration of granules, weakening amylose-emylopectin. bonds and_ increasing aniylose water interactions (Dist Li, Ovedel, Oyeyinka, & Ma, 201°), Most of the literature suggests that SP and solubility are lowered in HMT-treated starches (Hoover, 2010), which the opposite to what was found in this rice Nour study. This might be related to the interaction of starch with other components in the four, mainly proteins and lipids (ela et al, 2021). thas een reported tha the severity of HMT derived changes depends on temperature, and is elated to structural reorgan zation, water restriction, and amylose lipid, amylose proven, and ‘amylose amylopectin interactions (ga & Mironoesa, 2019). Loi eta (2020) also found that heating temperature caused an inerease in the solubility of DHT-starch, especially sehen the temperature was higher than 190 °C as was cur ease. 4, Color characterises ‘The color values of the comtol rice Nour (native) and modified samples are shown in Table 1. In general, the heat treatment caused & slight, although significant, decrease of lightness (L* values), indicating tha che color ofthe treated samples (except at 3%, 13%, and 1536 MC, ‘which remained unchanged) beceme darker, mainly at 30% MC. Flou color is important in bakery products, mainly with regard to bread ‘rumb color; therefore, the darkening effect could be postive inthe ease ‘of white rice four products, implying that they are wholegrain or more sina to tational wheat bread (Raia Henares, 2009). The hue ) ‘of reated samples varie significantly with respect othe contro, but i diferent ways depending on the treated sample MC. ehanged to reddish in samples treated at 89% and 30% MG, and became yellowish at 386, 18%, and 1596 MC. Chroma (C*) inereased slightly i all treated samples, indicating that che treatment caused more vivid colors. A significant deereaseof lightness and increase of b* coordinate ‘were also reported for DHT modified rice starches by Si ot sl (2018) “The analysis ofthe differences of color between each modified sample ‘Smit of ome piysicochemial parameters of conto ative) Ao and microwaved ens trate at ferent moisture content (MC) mc) Veas09a 4664080 07 One oe retry) wari ieeiae SPigedm) 78450408 820 40 Sat r02seh —assdand aga sone 95-0 fer oO. 9b e fiaroiea —sasysaad Rad sagsbe RRA LORId REM F Ghat BADR DORR FOE Bcoroase — fasstaabe | Taeraasd AOS TOASE —RLOSTaAT —TaaROSSe TPN FORA Soo +0084 «a0 nM ct —««AARFOMe «AN Fhe SOOM aH TOMB — RDF HAN MC3}%, MCF, NGT3N, MC 15%, MC 20%, MC-30%: Rice Nous Hated at 3,8, 13,15, 20 and 30% oF mo ie content. AAC 9: apparent amylose content SP selling power: dns dry matter. 1+ a, b= CIELAB coor courses; C* Cass hs; AE: Dilference of color beeen each sample and the coatiol. PT: Pasting texperatre, PV: Peak veo Tough sos; BV: Breakdown viscosity, SV: Setback vscost; FV: Final coy. Data ate the meat standard deviation. Vales with ete in eomnoa in these Une ate not signin fren (p< 0.05).wr 41 aon 130851 4 2 » a od? : - be 10 Sa 2 FA f ab 3 fi | . E «f 3 a a Ge = a ab ab} 5 Be ella 4 = 2 0 o Como! 3% = 8% «13% «1S% 20% 3086, Sample Fig. 2. Hydation properties of MW tenet ce flows: WAC (water absorption capacity, wae Hour dy mater black) ane! WS (water slit nde, x sll solis/100g ny mate) ty) ace epeseted on the let Yas and WAT wate abwopsion inde, seen our dry ater (white) epreseaed ‘nthe ght aie The enor bars epresent the anda deviation ‘andthe contol, At (Fable 1), allows to conclude that she teatments did not markedly modify rie Nour color, given that AE was always below 5, Indicating thatthe color differences could not be visibly difereatiated (Garein-Viguera& Zafila, 2001). The low protein content of rie four may explain the low occurrence of the Maillad reaction (MR) duxing MW treatment. MR and caramelization ae the two reactions involved in ‘generating color during heat treatment. Both reactions depend on tem perature and water activity (Rufian-Henares ea, 2009). The formation of reducing sugars during the heat treatment (Rufian Henares et a, 2000) was probably favored by higher MC in the flour during MW treatment, and could explain the darker color ofthe sample treated at 20% MC. Viscosity (Pas) 200 400600 Pasting properties ‘Typlel pasting profiles ofthe native and the MW. rested ree Murs are illustrated in Fig. 3. The corresponding pasting data are given i "able 1. Now iniportant differences were observed betweet the sample teeated at 3% MC and the control flour. The miost relevant change ‘observed inthis sample was a decreas in PT (—1 °C): this was opposite ‘what happened inthe other treated samples, where PT increased from 4°C108 °C with respect to the control flour. DHT would break intr: or Iter molecular hyerogen bonds of starches, which would facilitate the swelling of starch granules (Lei eal, 2020; et al, 2013). A Indicates greater resistance 10 swelling and ruprure. The maximum 100 ‘Temperature (°C) 8001000 1400 1200 Time (s) ig 8. Pasng profiles of MW wea siee Nous. Coaiouous grey line epresets the ener sight Ya).Increases in PT were observed In samples treated at an MC of 895 (5.8 °O), under DHT conditions, and at 20% (45.7 °C) and 30% (-8°0), under HMT conditions. The treatments decreased the PV ofall modified samples, with dhe maxinan deerenses fund in the same MC ‘samples: 8% (~3796) <209% (~40%) <30% (580%), The treatments a 13% and 159% barely showed any differentiaions in PV and the ‘emnining pasting properties. According to Li et sl. (2013), excessive Iheat could soparate glycosidic linkages and disrupt hydrogen bonds, which could decrease viscosity. Lei etal. (2020) also concluded that DHT of starches t temperatures above 170 °C decreased the viscometrie profiles, probably due to partial thermal degradation of amylose and amylopectin molecular an erystaline structure. This could explain why the sample treated at 83% MC, which reached 173 °C, presented a lower PV than those at 13% and 15% MC. Inthe ease of MT, other authors ‘also reported a decrease In PV and BV dependent on treatment cond tons (ig Mlronens, 2019) BV decreased in al rated samples with respect t the control, with the lowest values observed forthe samples treated at MCs of 8% (69%), 2096 (~728), and 30% (89%). The low BV of treated flour indicates «higher stability of te swollen granules versus shear and heating (Villanueva, Harasym, etal, 2018). tn this study flours with low swelling capacity exhibited less decrease in vi. ‘cosity after reaching the maximum value. SV is sally associated with the potential for retrogradation in starches, and lowering it means that there is less chance for retrogradation (sng el, 2017). The SV wales (of 19% and 15% MC samples increased by 9¥6 and 13% with respect to the control, while the samples treated at 20% and 30% MC decreased by 1296 an 38% respectively. The drop in the FY ofthe sample treated at ‘30% MC, which was 339% lower than the control sample, sigested that short term (amylose) retrogradation could be decreased by the MW treatment under these conditions. The results obtained revealed that the pasting parameters did aot show a regular evolution with MC as te Ported for other starch systems (rasoveanu & Nema, 2014 86. Rheolegical properties of gels obtained from treated flours ‘The rheological properties of gels made from MW treated rice four ‘were determined and compared to those of the gel made from the con trol (untreated) flour using dynamie oscillatory tests. Table 2 presents the parameters obisined from fitting the power law model to the fe ‘quency sweep data, the micxiniim tess (tng) within the LVR, as well as the stress at whieh the gels passed from sol ike «0 viscous ike Dehavior (G' =" and tan 8 = 1). ‘The oscillatory test evealed that MW treatment affected the rice flour gl vscoelastte modu regardless the M1 of the four during the table 2 wr 41 aon 130851 treatment (Pg. ). The gel made rom rice Nour treated at 3% MC dd not resent significant diferences fom the contro ice flo, except forthe “aun Which increased from 315 Pato 435 Pa. This indletes that atleast, the resistance of the gel to aisuption was significantly improved as 8 result of the treatment. the rest of samples, al viscoelastic properties showed significant differences with respect to the control (Fable 2). The ‘ost marked effect was observed on the sample treed at 8% MC, closely followed by that treated at 20% MC. Storage (6) and loss (G",) ‘moduli inereased markedly with MW treatment wit regard to the native ‘our following the order (he increase in G', and G",, rspeetively, with ‘regard to the control is shown in parentheses): 836 (4.66%, +466) = 2086 (461%, +4986) > 3096 (+354, +82%) ~ 15% (+446, 42686) = 19% (3696, +2190. The elastic modulus always increased more than ‘the viscous one, explaining the decrease in the loss tangent (G"/G') with MW treatment. "The values of G', were only slightly dependent on fe ‘quency, 28 the low “a” exponents(0.05-0.08) denote, sgaleanty Tower in ges made rom microwaved flours. This confirms that their sructre ‘was more stable explained bythe significantly higher elastic modulus of treated samples, The rate of increase of G" with frequency (°" exponent range: 0.26-0.31 was five ties that of’, which indicates that the loss tangent (6°'/G} increased signifiantly with frequency (with “e* valwes in the 0.20-0.23 range). The (tan 6); decreased slightly in treated samples, fom 0.120 010, which meas thatthe MW treatnent yielded sels with more pronounced slid like behavior. The tas and cross-over point shoved their maximum values fr the gels obtained from rice flour tweated at 8% MG (60% higher than the control ge). Both values ‘decreased with inereasing MC of the four during MW treatment. This confirms that DHT leads to the most stable and consistent and the strongest gel structures. Similar resus were obtained by other authors ‘when DICT vas apple to normal and waxy corn starches (Leal, 20205 Qi) eh, 2015), when diferent starches were treated with traditional HMT processes (Hoover, 2010), or when rice starch was treated by MW radiation (Villanueva, De Lan, et al, 2018). Comparing both conditions, we can conchide tha the rheological properties of the gel wore more affected by DHT than by HMT and that, within the later, the 20%6 MC generally led to greater changes than the 20%. 8.7. Gelasinization and rerogradation properties ‘The gelatnization enthalpy of native and microwaved! samples Is shown in isle 2- slight, not significant, derease inthe gelatinization enthalpy was detected in samples treated from 3% t0 15% MC. However, Jn samples treated at 20% and 305% MC the gelatinization enthalpy decreased 549% and 658, respectively, in reference co thar of native fer of treatment onthe heologieal properties and etrogredation degree in seven daysafric Nour els made fom native (contol our and microwaved ours treated at ferent moisture content (MC) end Nom owe Cae nee eam care cr wa4 waste Ta ee ‘ae ri0b wera Tiaras rovers . Gio +0004 Gars FOor2e4 ms) oma BGS FO.NIZK AMS FCOIOAD OGD +00 ab HOD + ON ab oven sraze Sente sate ase Tate fuse wine Can, 0120 400m G20 Foo01e O40 +0001e LO HOOSab 040s +0010 O10 F00N2eb O45 =D012e : S20 Loon az iomee aid saomae Oats Lomdsh 9210 L004 2M LOMSe nis L001 wb Emu) distise | Goaad Sac 3 tei ioe tariee Seah srize Ali (iedm) 9054027 77 40%5e $47 e006 fisoive — Aeasaah «te ozs eGo otese eoste vaste faise iui wine IC 3%, MEBs, ME 13%, MC 15%, MC 298, MCSORE Rice ow Leated at 3, 8 13, 15, 20 and 30% of molstae content The power aw model was Fed ‘expert esls ows quency sweeps. = Gras" — Gta ~ (a 5) a). ta), was obtained Kom the qotient Gy /G'at and homba GG", ‘and (an) tepeset the caste ad viscous modu nd the loss angen at eueney of Ha The, bande exponents quant the dependence degre of djaunie odul nd he loss angen with the exllaconfequency. ° Fiting region coefclet. aq taxi sree that samples can oerate nthe LVR, DR (3) = 1O0-Attet/Atigel. lige, Alt eltng enthalpy of ersalized amylopectin dung the gelatzation and vetioradation sane rexpetively; dy mater, Data fret mean standard deviation (0 =2), Vales with eter I conunon inthe save lie are nx signify aiferent (p= 0.05)wr 41 aon 130851 1000 100 10 A Il 0 1 10 100 1000 Shear strain (%) 1000 100 é & e lo lo Frequeney (Hz) Fig. Stxn eps (A) and iequeney sweeps (B) of gels preps with contol ee flour (=) 8% HI and 30% (4) MWtreate ce Hous. represented by full symbas presented by empey smbols. flout. Ths denotes » partial getatinlzation of these two flour samples uring the MY creatment. Retrogradation col be categorized into two processes: the gelation ‘of amylose solubilized during gelatinization, which happens in a short, period of time (minutes hours; andthe reerystallization of amylopectin, Which takes significantly laiger (7-10 days) (Ploypetcara, Suwanne por, Pochyen, & Gohan, 2015). Amylopeetn retrogradation ean be considered as a ime- and temperature dependent polymer rerystal zation process. The melting enthalpies of retrograded amylopectin in treated rice flours after 7 days of storage at 4 °C were recorded and ‘compared to that obtained in the contol (untreated) flour. No signif cant differences were observed in rtrogredation enthalpy, which was 95.7 J/g do in all samples, which denotes thet the ability of amyto pectin t0 reassociate after gelatinization was not altered by the MW "weatment. However, the degree of rettogradation (DR) changed in some ‘of them (able 2). For the contol flour and fouss treated at 33, 855, 1396, and 15%, the DR was 60-74%, with no signiiean diferences among them, Hossever, in the 20% aad 30% MC samples the DR values ‘wore 12496 and 1678, respectively, as result of the partial gelatinization ‘caused by the high temperature and moisture level during the treatment ofthese samples.4. Conclusions [MW created freeze dried ree our (39% MC) showed no change from native flour in techn fanetional properties. However, che four treated aC 8% MC showed important changes in the hydration and pasting properties studied and le to the most consistent and resistant gel. This ‘mall amount of water (lightly above the monolayer MC) was sufficiet to absorb MW radiation and to exert a plasticizing effet for the mo- lecular rearrangements of starch, responsible for these changes. The lowest peak nnd breakdown viscosities nnd the highest pasting tem peratures were found in the samples treated at 30%, 209, and 898 MC. DSC revealed thatthe flours treated wt 20% and 30% MC were partially pregelatinized, while the low MC of the remaining samples prevented ‘granular disruption. MW treatment Ineteased the WAC and SP of treated Nourse also increased the solubility of fours treated at 886 and ‘80% MG.'The significantly higher AAC ofthese wo samples with respect, to that ofthe control four could explain these results and confirm the highest severity ofthe treatment under these nwo conditions (he highest temperature and the highest MC), ‘The siidy shows that the MC of the Mlour during MW creatment makes it possible to modulate the echo unetional properties of the MW-moditied flour and the ricological and ermal characteristics of the gels obtained from them, being the MC of 8% the most effective in these changes. These MW-trested rice flours can be used in the pro ‘duction of food products with tailor-made functional properties stable for the elise population Author contributions Angela GarelaSolaesa and Felicidad Ronda conceived and designed the experiments; Analyzed aud interpreted the data; Contributed re ‘agents, materials, analysis tools or data; Wrote the paper. Angela Gaeta Solaesa, Marina Villameva performed the experiments; Analyzed and Interpreted the data. Jose M. Muior designed experinents and equip ‘ment used in the study and interpreted the results. Flicidad Ronda: Funding acquisition, Concepnualization, Methodology, Resources, Investigation, Visualization, Supervision, Writing - review & editing, Projet edministration. Declaration of competing interest “The authors confi that they have no conflicts of interest wi respect to the work described in this nsanuserip. Acknowledgements, “The authors thank the Ministerio de Eeonomia y Comypetitividad and the European Regional Development Fund (FEDER) (AGL2015 63849. (2.2), the Ministerio de Ciencia e Innovacién (P1D2019-110800RB 100), and the Junta de Castilla y Leén/FEDER VAO72P17 and VA195P20 {or their financial support. The authors thank Mr. Agustin Martin forthe 4esign and construction ofthe Teflon containers. M. Villanueva thanks References Ae: (1990) AACE ema mao, 44.19.01. Mace Ar On math AAC “ntoatonlaroced mato onion teas sotaee Ate, Calla, Rods 18). eet of vay pea partes stapes Rar 080208 Nan a Abeie,,& Renda F205), Poway, mole sro nd teal pope of te eeprom (ace) iol Sou ral of Cr Sec 19 20 Myc encmyiotenerjee amiss wr 41 aon 130851 eles, JN. (201), Pye modicadons of atch a Cape 5 starch fat ‘Sacre finn and plato pp. 225-259), i ues Io007 s7e9 150 rareanu M.& Nena, MB. (2010, Behaviour of tach expord te mire ‘ein xm Sans, 4s oda, 0. 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