Albert J.J. Woortman, Peter A.M. Steeneken Thermoreversible particle gels based on physically modified starch

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1 Albert J.J. Woortman, Peter A.M. Steeneken Thermoreversible particle gels based on physically modified starch TNO Nutrition and Food Research Stärke-Tagung, Detmold, April

2 TOPICS FOR TODAY Phase transitions in starch water systems A novel thermoreversible gelling starch Lab-scale products: structure and properties Effect of starch source Pilot-scale products: two types Applications: some examples Stärke-Tagung, Detmold, April

3 PHASE TRANSITIONS IN STARCH-WATER SYSTEMS Starch shows 3 phases when heated in water Semi-crystalline state Amorphous granular state (semi-crystalline structure disrupted; granule individuality preserved) Molecular dissolution state Phase transitions are C dependent phase diagram Stärke-Tagung, Detmold, April

4 PHASE TRANSITIONS IN STARCH-WATER SYSTEMS Starch applications are related to phase diagram This motivated us to explore phase diagram of potato starch Thickening agents Semi- Gelatinised Dissolved crystalline Melted Destructurised Noodles and pasta Chemical modification Bakery products Chemical modification Expanded products Bioplastics Temperature Stärke-Tagung, Detmold, April

5 PHASE TRANSITIONS IN STARCH-WATER SYSTEMS Method DSC at different starch water ratios to different final temperatures After cooling (and storage), DSC reheating and microscopy Stärke-Tagung, Detmold, April

6 A NOVEL GELLING STARCH Observations on 20 % potato starch when heated to C 1 0,9 0,8 heat flow [W/g] 0,7 0,6 0,5 0,4 170 C 0,3 62 C 0,2 0, temp [ C] Upper curve: First DSC heating scan of 20 % potato starch to 200 C Lower curve: Second heating scan after 20 h storage at 20 C Stärke-Tagung, Detmold, April

7 A NOVEL GELLING STARCH Figure 1. Photo micrograph (crossed polars) of Spherulite morphology of 20 % potato starch after heating to 200 C and overnight storage at 20 C. Texture was ointment-like The work-name Retrogel was adopted for both fresh and dehydrated gels Stärke-Tagung, Detmold, April

8 A NOVEL GELLING STARCH Thermoreversibility of 20 % gels Gels were prepared by heating ( C) and cooling 20 % potato starch in DSC cups. Heating temperature in subsequent heating / cooling cycles was 100 C. Gel melting peak temperatures ranged between C. Heating (to 100 C) / cooling (to 20 C) cycle Ageing time at 20 C Final heating temperature ( C) Melting enthalpy (J/g) Paselli SA Stärke-Tagung, Detmold, April

9 LAB-SCALE PRODUCTS: STRUCTURE AND PROPERTIES Preparation method 20 % Potato starch was heated in a stainless-steel tube at 10 C/min After cooling and overnight gelation, the gel was dehydrated with ethanol 170 C Temperature profile during heating Stärke-Tagung, Detmold, April

10 LAB-SCALE PRODUCTS: STRUCTURE AND PROPERTIES Gelation kinetics at 20 % and 20 C G' [Pa] tim e [h] Top to bottom: Retrogel 190 C, Retrogel 185 C, idem cold suspended, Paselli SA2, White dextrin B1102 Stärke-Tagung, Detmold, April

11 LAB-SCALE PRODUCTS: STRUCTURE AND PROPERTIES Molecular structure Product Preparation scale Final temperature ( C) M w (x 10-3 ) Potato starch ~ 100,000 Retrogel DSC Retrogel DSC Retrogel DSC Retrogel Tube Retrogel Tube Paselli SA2 270 White dextrin B Weight average molar mass (M w ) depends on final heating temperature. Even high-m w Retrogels contain maltooligosaccharides as small as glucose. However, at a comparable M w these amounts are smaller than in Paselli SA2. The branching pattern is not altered with respect to the parent starch. Stärke-Tagung, Detmold, April

12 EFFECT OF STARCH SOURCE Starch Amylose content (%) Final temperature ( C) C (%) G after 16 h (Pa) M w (x10-6 ) Tapioca Maize High-amylose maize Potato n.d Heating and cooling of waxy maize starch did not produce gels Stärke-Tagung, Detmold, April

13 EFFECT OF STARCH SOURCE Gelation kinetics at 20 C Potato 20 % / 185 C (1); Maize 20 % / 180 C (2); High-amylose maize 10 % / 180 C (3); Paselli SA2 20 % (4); Tapioca 30 % / 180 C (5). Stärke-Tagung, Detmold, April

14 OVERVIEW OF RETROGEL CHARACTERISTICS Retrogel forms thermoreversible gels Gels have a particulate structure and are spreadable Gel moduli are much higher and induction times much shorter than for Paselli SA2 at comparable concentration Retrogel shows functionality in instant applications Retrogel is molecularly degraded starch. It is functional over a wide range of M w : ~ Retrogel can be made from various starch sources. Gel moduli correlate roughly with amylose content Stärke-Tagung, Detmold, April

15 PILOT-SCALE PRODUCTS: TWO TYPES Process 20% potato starch suspension ph 5,5 jetcooking with 18 L / hour 160 sec at ~ 185 C cooling to ~20 C overnight stirred gelation desintegrate direct hot transport Spray drying Retrogel O Spray drying Retrogel S Stärke-Tagung, Detmold, April

16 PILOT-SCALE PRODUCTS: TWO TYPES Textures Retrogel O Retrogel S - M w = 2.1* M w = 1.8* High-modulus type - Spreadable type Stärke-Tagung, Detmold, April

17 PILOT-SCALE PRODUCTS: TWO TYPES Thermal transitions in gels 58 C 120 C 58 C 120 C 62 C These high molar mass Retrogels exhibit a small endotherm at 120 C that points to the melting of an amylose phase Stärke-Tagung, Detmold, April

18 PILOT-SCALE PRODUCTS: TWO TYPES Gelation kinetics % O G' [Pa] % O 20 % S 10 Paselli SA2 Gelation at 20 C after cook-up time [h] Retrogel O gels have a high modulus, which enables their use at a lower concentration Retrogel S has a modulus comparable to Paselli SA2 but a much shorter induction time Stärke-Tagung, Detmold, April

19 PILOT-SCALE PRODUCTS: TWO TYPES Spreadability 8 % O at 4 C 20 % S at 20 C G G tan - Spreadability is measured as a breaking strain in a dynamic strain sweep - Comparison of gels of similar modulus - Retrogel S exhibited a smaller breaking strain, i.e. had the better spreadability Stärke-Tagung, Detmold, April

20 PILOT-SCALE PRODUCTS: TWO TYPES HTST-treatment 5 min. 120 C. 5 min. 140 C. = 50 µm 10 % Retrogel S stored overnight at 20 C HTST-treatment of Retrogel S in water resulted in a gel with a rubber-like texture This result was not observed with Retrogel O Stärke-Tagung, Detmold, April

21 APPLICATIONS: SOME EXAMPLES Grated chocolate 17.2 % Retrogel O Low-fat vanilla ice cream 16.7 % Retrogel S Stable cuttable pudding 5.1 % Retrogel S HTST-treated Stärke-Tagung, Detmold, April

22 OVERALL CONCLUSIONS Heating of semi-dilute starch water systems into the solution state can be used for the manufacture of starch products that form thermoreversible spreadable particle gels (Retrogels) Products with different properties are obtained when processing conditions are varied - Heating Hot spray-drying Retrogel O (high-modulus type) - With intermediate gelation step Retrogel S (high-spreadability type) - HTST-treatment of Retrogel S Retrogel S-HTST (rubberlike type) Exploration of the phase diagram starch water may lead to the discovery of novel starch modifications Stärke-Tagung, Detmold, April

23 COOPERATION This research was done within the framework of Agrobiokon, a cooperation between Hoofdproductschap voor Akkerbouwproducten, AVEBE, and TNO Many thanks to: TNO I. Capron, C.F. de Ruijter, P. Sanders M.M. van Binsbergen, W.P. Vernooij, T.V.P. van Gestel Molecular characterisation Application research AVEBE J. Krikken, J. Aten, R. Voogd, A. van der Vegt Pilot-scale experiments: support and equipment Stärke-Tagung, Detmold, April

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