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8 FOOD POLYMER SCIENCE OF STARCH STRUCTURAL ASPECT FRINGED MICELLE MODEL OF PARTIALLY CRYSTALLINE STARCH AMORPHOUS REGION GLASS TRANSITION AT Tg FUNCTIONAL ASPECT STARCH MAP CRYSTALLINE REGION MELTING TRANSITION AT Tm

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11 CORRECTION AND COMMENTS FOR BLANSHARD'S CONCEPTUAL GLASS CURVE Tg', Wg' CURVE SHOULD PASS THROUGH Tg', Wg'

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20 INGREDIENT SELECTION FOR STRUCTURE & FUNCTION WATER & FOOD MONOMER OLIGOMER POLYMER COMPONENT IN EVERY CATEGORY SUGAR ALCOHOLS STARCH AMYLOSE GLUTEN GLUTENIN POLYDEXTROSE STARCH AMYLOSE STARCH AMYLOPECTIN GLUTEN GLIADIN GLUTEN GLUTENIN RESISTANT STARCHES

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29 RELATIONSHIP BETWEEN GELATINIZATION TEMPERATURE AND EXTENT OF CRYSTALLINITY OF NATIVE GRANULE GELATINIZATION TEMPERATURE IS Tg OF AMLYOPECTIN DECISIVE FACTOR FOR EFFECTIVE Tg IS EXTENT OF MOBILITY OF AMYLOPECTIN BRANCHES GELATINIZATON IS A CONTINUUM OF NON-EQUILIBRIUM RELAXATION PROCESSES KINETICALLY CONTROLLED BY EFFECTIVE INSTANTANEOUS Tg ΔT = T - Tg inst ΔW ==> ΔT [Slade (1984)]

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31 EFFECT OF WATER CONTENT ON THERMAL BEHAVIOR OF STARCH NORMAL RICE STARCH AT 10-80% MOISTURE CONTENT DSC heat flow curves of native rice starch at various water contents: A) starch with "as is" moisture of 10 w%; B-F) starch with water added to water weight fractions indicated. Reproduced, with permission.

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43 LOCATION OF TEMPERATURE RANGES FOR GELATINIZATION, ANNEALING, MELTING, NUCLEATION, AND RETROGRADATION PROCESSES

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60 STANDARD TACO SHELL PROCESS DSC PROFILES

61 PRODUCTION OF CORN MASA IS A 2-STEP PROCESS

62 ROLE OF LIME NOT FOR GELATINIZATION NO EFFECT ON AMYLOPECTIN

63 ROLE OF LIME ENHANCE PASTING OF AMYLOSE AND RATE/EXTENT OF WATER UPTAKE

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73 FOOD POLYMER SCIENCE DESCRIPTION OF STARCH RECRYSTALLIZATION/RETROGRADATION/STALING RECRYSTALLIZATION OF AMYLOSE DP 15 TO 35 MOBILITY NOT LIMITED AND DP < FOLD LENGTH

74 DP ~ 3000

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81 STEADY-STATE! BUT NOT EQUILIBRIUM RH INVERSELY LINEAR WITH Tg AND CRISPNESS

82 ANOTHER EXAMPLE OF REAL TIME EVENT AT ~ 20C ABOVE Tg = Tg

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85 BETTER TO SAY FROZEN OR UNFROZEN IN REAL TIME

86 BETTER TO SAY FROZEN OR UNFROZEN IN REAL TIME

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90 DSC ANALYSIS OF STALING IN BAKED GOODS DSC heat flow curves illustrating the rate and extent of starch recrystallization in two types of commercial baked goods: A) white bread, immediately after baking (upper curve) and after 1 week at room temperature (lower curve); B) English muffins, on days 1 (upper curve), 7 (middle curve), and 13 (lower curve) after baking.

91 ACCELERATION OF STALING OF FRESHLY BAKED BREAD CRUMB A B C D DSC heat flow curves of freshly baked white bread crumb staled at different storage temperatures and times: A) 25C for 39 days; B) 25C for 42 hours, then 40C for 2.5 hours; C) 0C for 42 hours, then 40C for 2.5 hours; D) -11C for 42 hours, then 40C for 2.5 hours.

92 CREATION OF STARCH NETWORK OPTIMUM CONDITIONS = SAMPLE G DSC heat flow curves of wheat starch:water 1:1 mixtures, stored under different T/time conditions immediately following gelatinization: A) 40C for 4.5 hr; B) 25C for 3.5 hr; C) 4C for 3 hr; D) -23C for 2.5 hours; E) -196C for 1 min, then -23C for 2 hr; F) 25C for 2 hr, then 40C for 5 hr; G) 4C for 2 hr, then 40C for 6.5 hr; H) -23C for 2 hr, then 40C for 6 hr; I) -196C for 1 min, then -23C for 2 hr, then 40C for 5.5 hr.

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94 EFFECT OF INCREASED NUCLEATION TIME DSC heat flow curves of wheat starch:water 1:1 mixtures, nucleated for different times at 0C, then propagated for 30 min at 40C, immediately following gelatinization: A) 10 min; B) 30 min; C) 60 min; D) 180 min; E) 240 min; F) 300 min.

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99 Molecular Weight

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112 THEORY CASE STUDY PRACTICE GOAL TO CREATE A UNIQUE RESISTANT STARCH WITH THERMOMECHANICAL STABILITY IN BAKING AND EXTRUSION PROCESSES NEED CRYSTAL MELTING ABOVE 140C AT HIGH WATER CONTENT NEED TO AVOID RECRYSTALLIZATION OF TYPICAL STALED STARCH (Tm ~ 60C) AND AMYLOSE-LIPID CRYSTALS (Tm ~ 110C)

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114 What is Resistant Starch? RS 1 Physically inaccessible starch (mainly occurs in partly milled grains and seeds) RS 2 RS 3 Enzyme resistant raw starch granules (present in raw potato and banana) Enzyme resistant recrystallized starch (familiar recrystallized starch is the retrograded, "staled" starch of cooked potatoes and bread after cooling to room temperature or below) RS 4 Enzyme resistant starch that is created by chemical modification

115 Why is X150 Resistant Starch Good for You?.. one of the major developments in our understanding of the importance of carbohydrates for health.. has been the discovery of resistant starch (Report of the joint FAO/WHO Expert Consultation in Rome, p , April 1997) Important physiological effect of resistant starch is its fermentation in the large intestine (Gordon, D.T., et.al., Resistant Starch: Physical and Physiological Properties 1997) Fermentation gives rises to: Lower colon ph (protects against cancer) Increased fecal weight or bulk (full feeling; satiety) Potential to slow blood glucose rise and glycemic load of foods Analyzes as total dietary fiber with AOAC method (IOM report Dietary Reference Intakes Proposed Definition of dietary Fiber 2001, several methods, including AOAC method , , , , , , and , are characterized as officially accepted, although no formal statement from the FDA

116 X150 is a Unique RS 3 Heat-stable with a melting point of 150C Superior baking characteristics Low water-holding capacity Browning Crisp texture 50% insoluble fiber by AOAC Method ; therefore is calorie-reduced Functions as a flour replacement ingredient in wide range of grain-based products

117 X-150 Resistant Starch Patent Estate Inventors: Haynes, L., Gimmler, N., Locke, J.P., Kweon, M., Slade, L., and Levine, H PCT Int. Appl. WO 99 22,606. Process for making enzyme-resistant starch for reduced-calorie flour replacer U.S. Patent 6,013,299. Process for making enzyme-resistant starch for reduced-calorie flour replacer U.S. Patent 6,352,733. Enzyme-resistant starch for reduced-calorie flour replacer U.S. Patent 6,613,373. Enzyme-resistant starch for reduced-calorie flour replacer U.S. Patent 7,531,199. Process for making enzyme-resistant starch for reduced-calorie flour replacer.

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122 AACC Wire-Cut Cookie Test Baking with High Quality Biscuit Flour and 50% Replacement of Flour by Nabisco Patented X-150 and National Starch Commercial RS Ingredients Climax Flour 100% X % Hi-Maize % Novelose % Novelose % 17 April 2003 INVERTED SHOULDER