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Carbohydrate Research 346 (2011) 2727–2735

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Structural and physicochemical characterisation of rye starch
S.V. Gomand ⇑, T. Verwimp  , H. Goesaert, J.A. Delcour
Laboratory of Food Chemistry and Biochemistry, Leuven Food Science and Nutrition Research Centre (LFoRCe), Katholieke Universiteit Leuven,
Kasteelpark Arenberg 20, B-3001 Leuven, Belgium

a r t i c l e i n f o a b s t r a c t

Article history: The gelatinisation, pasting and retrogradation properties of three rye starches isolated using a proteinase-
Received 23 May 2011 based procedure were investigated and compared to those of wheat starch isolated in a comparable way.
Received in revised form 20 September 2011 On an average, the rye starch granules were larger than those of wheat starch. The former had very com-
Accepted 22 September 2011
parable gelatinisation temperatures and enthalpies, but slightly lower gelatinisation temperatures than
Available online 29 September 2011
wheat starch. Under standardised conditions, they retrograded to a lesser extent than wheat starch.
The lower gelatinisation temperatures and tendencies of the rye starches to retrograde originated prob-
ably from their higher levels of short amylopectin (AP) chains [degree of polymerisation (DP) 6–12] and
Rye starch
Wheat starch
their lower levels of longer chains (DP 13–24) than observed for wheat starch. The rapid visco analysis
Amylose/amylopectin fractionation differences in peak and end viscosities between the rye starches as well as between rye and wheat
Amylopectin structure starches were at least partly attributable to differences in the levels of AP short chains and in average
Gelatinisation amylose molecular weight. The AP average chain lengths and exterior chain lengths were slightly lower
Pasting for rye starches, while the interior chain lengths were slightly higher than those for wheat starch.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction therefore well documented. In contrast, relatively little has been
published on the isolation and properties of rye starch.
Rye products have a high nutritional value, especially when Starch consists of a mixture of amylose (AM) and amylopectin
they contain wholemeal rye flour because of their considerable lev- (AP). Typical levels of AM and AP in cereal starches are 22–28%
els of dietary fibre, vitamins, minerals and phytoestrogens.1 Starch and 72–78%, respectively, although, for starches of some botanical
is the major rye reserve carbohydrate, but only limited information sources, also high AM (up to 70% AM) and waxy (<1% AM) geno-
is available on either its physicochemical properties or its struc- types exist.3 Some minor components commonly associated with
tural characteristics. Rye starch can be isolated from rye flour by rye starch include lipids (0.4–1.7%), proteins (0.1–1.3%),4 phospho-
alkaline extraction or Pronase-based procedures.2 Wheat, maize, rus (0.03%) and other minerals (0.4%).5
potato, cassava and rice starches are industrially isolated from AM is an essentially linear polymer consisting of a-D-glucopyr-
their parent cereals and function as thickening, stabilising or filling anosyl residues linked by a-(1?4)-bonds with few (<1%)
agent. Their composition and physicochemical properties are a-(1?6)-bonds.6 It has an average degree of polymerisation (DP)
in the range of 500–6000.3 AM can form helical inclusion com-
plexes with lipids and has a reported molecular weight (MW) of
about 2.2  105.5 AP is a highly branched polymer consisting of
Abbreviations: AP, amylopectin; AM, amylose; CL, average chain length; BV, blue a-D-glucopyranosyl residues, linked by a-(1?4)-linkages with
value; Tc, conclusion temperature; Tc,retro, conclusion temperature of retrograded
5–6% a-(1?6)-linkages.3 It has a DP ranging from 3  105 to
amylopectin; DP, degree of polymerisation; dm, dry matter; DSC, differential
scanning calorimetry; DHretro, enthalpy of retrograded amylopectin; ECL, exterior 3  106 (Ref. 7) and a MW of 1  107 to 1  109.3 Several authors
chain length; HPAEC, high-performance anion-exchange chromatography; HPSEC, reported the presence of molecules intermediate between AM
high-performance size-exclusion chromatography; DH, gelatinisation enthalpy; ICL, and AP in starches from botanical origins including wheat,8 pota-
interior chain length; IM, intermediate material; kmax, iodine binding wavelength to,9 wrinkled pea,10 rice,11 high AM maize12,13 and oat.14 In rye
maximum; BL, long B chain residues; DHaml, melting enthalpy amylose–lipid
complexes; MW, molecular weight; To, onset temperature; To,retro, onset temper-
starch, intermediate material (IM) also occurs.8,15
ature of retrograded amylopectin; Tp, peak temperature; Tp,retro, peak temperature Several methods have been used to fractionate starch into AM,
of retrograded amylopectin; PAD, pulsed amperometric detection; rt, room AP and, in some cases, IM. Two main methods currently used are
temperature; RVA, Rapid Visco Analyser; BS, short B chain residues; SEC, size- aqueous leaching and selective precipitation. In the first method,
exclusion chromatography; WAXD, wide angle X-ray diffraction.
⇑ Corresponding author. Tel.: +32 16 321582; fax: +32 16 321997. AM can be selectively leached from starch granules during heating
E-mail address: (S.V. Gomand).
in aqueous media slightly above the gelatinisation tempera-
Present address: Natra Allcrump, Nijverheidsstraat 13, B-2390 Malle, Belgium. ture.16,17 At higher temperatures, in addition to AM, AP is extracted

0008-6215/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.

enthalpies (DH) and AM–lipid complex enthalpies (DHaml) were Potato and Starch Technology. Belgium).20 respectively. Sydney.2 However. The starches because it had the highest crystallinity. 52% and 63% mine the level of starch retrogradation. the starch granules are first completely dispersed in hot water and discarded. They 2. setback (the material was passed through a 38-lm sieve with additional difference between the viscosity at the end of cooling and the . 2. only limited infor.24 using a commercial wheat starch (Meriwit ical behaviour of the starch and hence was an objective of the pres. AM content was determined by the structure of starch is important for explaining differences in phys. Analyses were performed at least in triplicate. The gelatinisation temper- produced by milling rye or wheat at a moisture level of 15% or ature range was calculated as Tc To. we evaluated differences in physicochemical ibration. an adaptation of the AOAC which hence precipitate.2 supernatant by freeze drying or by precipitation with alcohol. The remaining supernatant may contain IM. Bray.retro) temperatures. Bergthaller (Institute for Cereal. The crude starch AP less soluble and increases AM yields. gelatinisation viso) were provided by Prof. 6 °C).3. / Carbohydrate Research 346 (2011) 2727–2735 and an additional purification step is required.5. followed by a second heating to deter- laboratory mill CD1. Elt. chemicals and enzymes used were of at least der the same conditions as those of starch gelatinisation. Amylum.17 A second long and te. Gouda. The onset Three rye samples of different cultivars (Avanti. peak (Tp) and conclusion temperatures (Tc). It was then air-dried overnight and gently passed through a lar organic compound (such as thymol or n-butanol). their units (U) were as de- 2.5 mg/g original flour) was added. which can be recovered by precipitation with alcohol. containing 0. Starch (4. Structural features of was taken as 100%.4. The gelatinised samples were 16%. as is the tol acetates obtained after acid hydrolysis (120 min at 110 °C). b-amylase and pullulanase were obtained from Megazyme (Bray. Belgium). Materials and methods was added [1:2 w/w starch dm:water (dm: dry matter)].0 g) were subjected The isolation procedure was based on the method described by to the following time–temperature profile: equilibration for Morrison et al.retro). AM is then precipitated with a po. Materials were heated from 20 °C to 120 °C at 4 °C/min and an empty pan was used as reference. Dr. DE.1 M Tris– holding at 95 °C for 15 min. dious procedure gives more representative fractions. analytical grade and obtained from Sigma–Aldrich unless indicated otherwise. Australia). Where enzymes were used. Starch characterisation butanol–saturated water.2 It was performed without 2 min at 50 °C. respectively. Pretreatment of deionized water until no more starch was extracted. Total starch content was determined using a total starch test kit mation is available on its structural features. A proteinaceous layer was scraped off from the starch surface od.2728 S. Nikita and Tre- (To). Rye or wheat flour was suspended in 0.02% NaN3 temperature decrease to 50 °C and a final isothermal step at and 0.12. a cooling step (9 min) with a linear HCl buffer [pH 7.00– 6. wide-angle X-ray dif- this end. This setup provided information on the relation. Starch gelatinisation and retrogradation ship between the structural aspects and the physicochemical prop- erties of rye starch.6. Germany). Detmold.22 Monosaccharide A PronaseÒ-based isolation procedure has been successful for compositions were determined by gas chromatography of the aldi- isolating starch from rye flour in high yields. Starch isolation procedure Visco Analyser (RVA-4) (Newport Scientific. France) stored for 14 days at 20 °C. W.16. 0. AM is then further purified by repeated recrystallisation from n. Belgium) with known AM content (26. to date. The peak viscosity (the maximum viscosity during Pronase E (0. New Castle. Differential scanning calorimetry (DSC) was carried out with a Q1000 DSC (TA Instruments. prior defatting. clean.18 tent was determined based on Morrison et al. Granule size distributions. In addition. Swelling and pasting behaviour were investigated with a Rapid 2. respectively.01 M disodium EDTA] (1:10 w/v) and stirred for 1 h at 6 °C. V. Starch suspensions (10% dm. 50 °C (10 min). the rye AM and AP were compared with those of the corresponding wheat polymers. The pans were hermetically sealed and equilibrated for at least 20 min. Calibration was with indium. 2. Yields of starch are ex- an insoluble complex with AM.14 An. The physicochemical properties of the rye starches were culate the relative crystallinity. 15 min. a Methods 44-19 and 08-01. and the suspension pasting). total weight 25.2. Wheat (variety determined using TA Universal Analysis software. Pronase E (Strep- ples was done under the experimental conditions also used during tomyces griseus) and isoamylase (Pseudomonas amyloderamosa) the first heating. Temperature Zohra) was obtained from AVEVE (Landen. IM and AP.19 and Verwimp et al. Treviso and Zohra. Ireland). Barley onset (To. The were purchased from Sigma–Aldrich (Bornem. In this meth. All reagents. Aalst. Rapid viscosity analysis fined by the respective suppliers. with a Chopin (Villeneuve-la-Garenne. Nikita.00 mg) was accurately weighed in an aluminum pan and water 2. starch was isolated from three rye samples of different fraction (WAXD) and viscosity behaviour of the rye and wheat origin by the above-mentioned PronaseÒ-based isolation proce. The AM contents are expressed as percentages of total and structural properties of starch of rye from different origins. 6 °C). Moisture and ash contents were determined based on AACC other approach to fractionate starch is the use of concanavalin A.5% (w/v) NaHSO3.1. obtained was suspended in water and centrifuged (1000g. Its relative crystallinity were then fractionated into AM. method of Chrastil. Protein contents were protein that binds to the non-reducing ends in the AP molecules determined using the Dumas method. Extraction rates were 52%. The combined starch with hot aqueous n-butanol before aqueous leaching makes washings were centrifuged (1000g. 55%. Total lipid con- concanavalin A and remains in solution. Flour was was expressed in °C and enthalpy in J/g. The concanavalin A–AP complex is then Official Method21 to an automated Dumas protein analysis system destroyed by hydrolysis with a protease. Heating of the stored sam- for Avanti. I. Gomand et al. peak (Tp. The Netherlands). Knowledge of the (Megazyme. 15 min. and the enthalpy (DHretro) of retrograded AP were determined un- Ireland). a linear temperature increase to 95 °C in 9 min. starches were studied using the methods in Verwimp et al. The AM binds very little (EAS varioMax N/CN.retro) and conclusion (Tc.23 case for its physicochemical properties. To starch contents. Nikita served as reference starch examined and compared with those of a wheat starch. which forms 250-lm sieve using a mortar and pestle. USA). breakdown (the difference between the peak viscosity was digested for 44 h at 6 °C under constant stirring. The digested and the viscosity at the end of the holding phase). This step was repeated until the starch was visually or aqueous dimethyl sulfoxide.0%) for cal- ent study.2 To cal- dure. AP can be recovered from the pressed as percentage of the total starch content of flour.

Preparation of non-granular starch Non-granular rye and wheat starches were prepared according Size-exclusion chromatography (SEC) of non-granular rye and to Klucinec and Thompson.1 M KOH.0 mL of 100% MeOH in a screw cap 1176 mL of 6. The HPAEC–PAD was performed with an ED-40 electrochemical . Debranching of rye and wheat AP was performed by the method The supernatant (AP III) was combined with the first two superna. The supernatant is tion (1000g. the temperature at which the derivative with an Ultraspec III UV–visible spectrophotometer (Amersham [d (viscosity) / d (time in min)] increased. 15 min. that is.0 M urea.000g.4  104. alcohol (1176 mL) was added.0 mL) of the gelatinized sample was added to 10 lL of 2. An ali- pellet was washed with 50 mL of 95% EtOH and again centrifuged quot (1.8  104.12 A sample (40 mg) the method described by Somogyi. 10 min). After centrifuga- cooled and centrifuged as described above. After centrifugation amyloderamosa isoamylase (625 U/50 lL of 600 mM NaOAc buffer (10. The residue (AM) was redispersed 5. Fractions 2.5 mL/min) using 50 °C for 24 h. IM and AP fractions was performed was dispersed in 200 mL 90% (v/v) DMSO by heating the mixture as described by Klucinec and Thompson12 with modifications.0% n-BuOH was added.27 respectively. an aliquot (1. After filtration and the pellet was washed by suspending it in 50 mL 95% EtOH.0 mL) was then placed in a 100-mL volumetric flask were determined by high-performance anion-exchange chroma- along with 95 mL of deionized water and 2. 4 °C). Size-exclusion chromatography of non-granular starches and starch fractions 2. 78.000g.1. 15 min.2  104.45 lm). All samples were scanned from 500 to 800 nm temperature (°C).6) at 37 °C for 24 h.0 mg KI/mL) was added. the mixtures were resuspended by 40. respectively. The supernatant (AP II) was combined with the first one. 2.73  104.38 mg of I2/mL and 0. Preparation of debranched amylopectins above.0 mL of an aqueous tography (HPAEC) with pulsed amperometric detection (PAD). 300 mL. 4.0 g. Japan) with peak MWs of 160. After centrifugation (10. I2–KI solution (2. IM and AP fractions were determined in triplicate according ends were analysed by the phenol–sulfuric acid method26 and to the method of Klucinec and Thompson. 700. degassed 0. 5. cooled and centrifuged as 2.6.2% of both n-BuOH and isoamyl alcohol (300 mL).6.8. Total carbohydrate level and content of reducing AM.6. Fractionation was followed by centrifugation (6500g.0 mL) of each SEC fraction was neutral- on the method of Klucinec and Thompson12 with slight modifica. The AM was suspended in deionized water (w/v) sodium azide and hydrolysed with Pseudomonas amylodera- and lyophilized.0 mL of deionized water with intermediate and final centrifuga- in 120 mL 90% (v/v) DMSO and AM was precipitated with 280 mL tion steps as above. The BV was the extinction Viscosity measurements were carried out in duplicate and the at 635 nm under the above experimental conditions. in a solution containing 5. 2.0 M KOH) for 8 h under mild magnetic stirring and then centrifuged (6500g. The precipitate was then dried at macia Biotech) in an ascending mode (flow rate 0.0% dm suspensions were determined. 300. and the sample was cooled to RT. diluted to 10.0 mL with deionized water. Following sample (15 mg) was dispersed in 1. 11.0 mL of iodine solu- tions. period of 18 h. and the mixture was phase (1. Detection was with a differential refractive index detector (RID-10A. 4 °C). AP and IM were then precipitated with (100 °C. 10 min). The pasting without sample. This mixture was heated. A in boiling water for 180 min with frequent hand shaking.10. Starch fractionation 2. 280 mL 95% EtOH was added.0% (6500g. The kmax difference between two measurements was less than 31 cP along was the wavelength (in nm) at which the extinction was the high- the whole temperature profile of the analysis. 15 min.0 M HCl and mixed with 5. An The branch chain length distributions of the rye and wheat AP aliquot (1. tube and incubated in boiling water for 10 min. 4875. 21. The residue was redispersed in 168 mL 90% (v/v) DMSO and (10. Pharmacia Biotech. and the residue was redispersed 2500. The enzyme was inactivated by heating evaporation to ca.0 mL of of 95% EtOH. (0.0 mL of concentrated mobile dispersion. Uppsala. Amylopectin average chain length and chain length distribution 2. 15 min. Amersham Phar- procedure was repeated once.7. The sample was resuspended in 5. 2. ized with 25 lL of 1. Japan). Blue value and iodine binding wavelength maximum of non-granular starches and starch fractions The average chain length (CL) of the isoamylase debranched rye and wheat amylopectin AP was determined by calculating the ratio The blue value (BV) and iodine binding wavelength maximum of the total carbohydrate concentration to the concentration of (kmax) of the non-granular rye and wheat starches and of their reducing ends. The mixture was heated.0 mg) was suspended in 3. 150 and 75. Tokyo. Control solutions were made in the same way but (cP)] of 10. Kyoto. was also determined. and then they were centrifuged (10.0  104. V. dry weight) wheat starches and of their AM. Non-granular rye and wheat starches were fractionated based To this end. AP tants. The residue was redispersed and centrifuged in the same way. was dispersed in 10. Shimadzu.000g. Sweden).6) at 37 °C for 24 h. 4 °C).9. The heating (100 °C. est over the range of the wavelengths. 4 °C).28  104 and shaking. 10 min. A solution containing 6. Gomand et al. of Umemoto and co-workers25 with slight modifications. An aliquot (6. the residue was washed twice with referred to as the IM fraction. The combined AP containing supernatants and mosa isoamylase (1250 U added in 50 lL of 600 mM NaOAc buffer the IM containing supernatant were each concentrated by rotary pH 4.0 mL of DMSO containing 10% 6.90 mg of KI/mL). / Carbohydrate Research 346 (2011) 2727–2735 2729 viscosity at the end of the holding phase) and final viscosity (the mixture was brought to 100 mL with deionized water and mixed viscosity at the end of the RVA run) [all expressed in centiPoise immediately. S. 1300. 4 °C). After cooling. 4 °C). Next. Finally. 4 °C). the sample was incubated again with P. incubated The column was calibrated with Shodex pullulan standards (Sho- at 95 °C for 60 min and cooled to room temperature (RT) over a wa Denko.2  104. 15 min.2. 350 mL and 250 mL of 95% EtOH.0 g) was dispersed in 168 mL of 90% (v/v) tion (0.0% of both n-BuOH and isoamyl measured at 620 nm. Starch fractionation (5.0 mL) were collected and their iodine binding was examined. The extinction was DMSO.0 mL of the filtrate was injected. the enzyme was inactivated by 95% EtOH followed by centrifugation (6500g.6 cm. AP and IM residues were suspended in deionized water and lyophilized. The supernatant was discarded. The washing with a Sepharose CL-2B column (74 cm  1. The supernatant (AP I) was saved.18  104 and corresponding to approximate DPs of 9875. 1.0 mg I2/mL and 20. 18 °C). the pellets were washed with 150 mL of pH 4. the AM deionized water and incubated in boiling water for 60 min.12 Granular starch (10. 15 min. 15 min. The mixture was stirred.

that described by Verwimp et al. USA) and an AS. DP 7) and 4 Shodex were normalized and divided into four fractions (F1 with DP 6–12. DP 1). and 400). The mixture was mixed. 20 °C).12. pH comparable to those obtained for the rye starches (Table 1). A second aliquot (0.07 0. 700.0 81. The rye and wheat starches were of high pur- of partially debranched b-limit dextrin. Shimadzu) 90% (v/v) DMSO.02 0. V) observed for rye cultivar Avanti. High-performance size-exclusion chromatography of debranched b-limit dextrins of amylopectins Yield 85.0) was added. The system was calibrated using and the eluent gradient programme were as described by Jacobs separate 50 lL injections of 8 separate solutions: glucose et al. The exterior chain length [ECL = CL  (b-amylolysis limit/ The sample was then incubated in boiling water for 10 min and re.05). USA). DP 5). Waltham.25 lm) and in. Regions I. 880 ered to represent long B chain residues (BL).11 0. The chromatograms of the debranched b-limit dextrins were divided into seven regions (I– The b-limit dextrins of rye and wheat AP were prepared using VII) based on the retention times of the minima (between regions the method by Klucinec and Thompson31 with slight modifications.10 0. IV (DP 7–22). / Carbohydrate Research 346 (2011) 2727–2735 detector (Dionex.5 index detector (RID-10A. USA) con- 3000 autosampler (Thermo Electron Corporation). An aliquot (0. cultivars Avanti. V. cooled to RT and centrifuged (5000g.12 HPSEC of debranched b-limit dextrins of rye and wheat AP was Total lipids 0. held overnight at 4 °C and subsequently cen- trifuged (250g. 4.2  104. III–IV. V–VI and VI–VII) and the inflection (between IV– AP (12. It was then incubated in boiling water tion procedure resulted in a higher starch yield for wheat (90.5 mL of 95% EtOH and once with 0.5 mL acetone. CA. This 4. Preparation of debranched b-limit dextrins of refractive index response at each time was divided by the MW of amylopectins the carbohydrate eluting at that time.02 M.05 dzu) connected in series to an injector (SIL-20A autoinjector. filtered (0. VI (DP 3) and VII the sample incubated at 50 °C for 48 h with constant agitation. DP 2).29 The relative amounts of AP chains (MW = 829. 10 min.1 mL) of each completely deb- Table 1 ranched b-limit dextrin was added to 200 lL of 100% DMSO and Yield and chemical composition (%dm) of the starches isolated from flour of the rye saved for analysis by high-performance size-exclusion chromatog.04 0. 75 and 36.5 mL/min) was an on-line degassed jected (20 lL) onto a CarboPac PA-100 anion-exchange column (DGU-20 A5. regions IV and V short lL. The starch yields ob- (50 °C. The solution was vortexed.5 83. maltopentaose molar PAD detector responses.5 mL) was mixed with NC. To this solution than for rye (80. They were main- prepared by adding 0. Shimadzu).0 mg) was dispersed in 120 lL of 90% (v/v) DMSO by heat. 25 U/mL in 0.06 0.21. 0.59  104 and corresponding DPs of ing to Hanashiro and co-workers. pullulan standards (Showa Denko) with MWs of 11.34 0.2730 S. The recovered b-limit dextrin was air-dried. The precipitated b-limit dextrin 3.43 performed based on the procedure of Klucinec and Thompson.25 mL of 1.4 and 24. In order to obtain molar-based chromatograms. 1.02 0. the differential 2.03 0. mobile phase (flow rate 0. The sample was incubated at 50 °C for 22 h with constant agitation.5 M NaOH to the isoamylase deb.06 0. Statistical analyses heated in boiling water for 10 min and cooled to RT.4 Ash 0.73  104. Gomand et al.11. 10 min.2 mL) was saved for b-amylolysis limit determination based on Pearson’s correlation coefficient analyses were performed (sig- the total carbohydrate26 and the reducing power27 of the solutions nificance level P <0. pH 6.0) was added. maltoheptaose (MW = 1153.02 M NaOAc buffer.30 ca.75) was added.9%). Shimadzu) which was operated at 40 °C. USA). Sunnyvale. injected volumes 50 lL) and a differential refractive Amylose 22. 0. DE.28 Individual peaks in the chromatograms were corrected for (MW = 180.5 mL of 95% EtOH. Nikita and Treviso and flour of the wheat cultivar Zohra raphy (HPSEC). Statistical analyses were conducted using [b-amylolysis limit (%) = 100  reducing maltose/total glucose ex. Detector responses and (250 mm  4 mm) in combination with a CarboPac PA-100 guard the resultant chromatograms were analyzed using LC Solution soft- column (Dionex). Samples were nected in series were used for the separations. The wheat starch contained 23. 300. Warm NaOAc buffer (50 °C. Results and discussion was washed twice with 0.43 ity as shown by the low ash. Shi. (Zorbax PSM 60S. Starch yield and chemical composition 1000g (10 min. protein.31 of the above b-amylase buffered solution was added.13. Rye starch Wheat starch Avanti Nikita Treviso Zohra 2. II (DP 50– (50 l lL. II–III. . Agilent Technologies. The mixture was tained for the rye samples were similar and in accordance with mixed.02 M NaOAc buffer. The ranched AP. at which time an additional 50 lL also calculated according to Klucinec and Thompson.36 0.2 For wheat. III (DP 22–50). the starch yield was Isoamylase solution (40 lL. the eluents ware (Version 1. tained at 50 °C using a column oven (CTO-20AC. 20 °C). a P-4000 gradient pump Two 30-cm columns packed with 6-lm porous silica microspheres (Thermo Electron Corporation. Wilmington.4 24. F2 with DP 13–24. pH 6.02 M NaOAc buffer. An aliquot (0. lipid and monosaccharide U/mL in 0. The AM content of the rye starches ranged be- was incubated at 37 °C for 24 h with constant agitation and then tween 22. DP in boiling water for 10 min and cooled to 50 °C. The sample contents (Table 1). pH 4.33 0. 1. Xylose 0.0%) for 10 min and returned to a water bath at 37 °C. The pulse potentials and durations. pH 4.2 24. 20 °C).18  104 and 0. Shima. pressed as maltose]. incubated B chain residues (BS) and regions VI and VII residues of A chains. Warm NaOAc buffer wheat flours and their chemical composition. Shimadzu). II and III were consid- ing in boiling water for 10 min.75) was added and the sample was incubated at 37 °C for 24 h is in contrast to earlier findings2 where the PronaseÒ-based isola- with constant agitation.0 mg) was mixed with 50 lL of 90% (v/v) Table 1 lists the yields of the starches isolated from the rye and DMSO and heated in boiling water for 10 min. incubated in boiling water for 10 min and cooled to 37 °C.02 madzu.5% AM. MA. 350 lL.75) was added. V (DP 4–7). The b-limit dextrin (3.9 23. 100) + 2] and interior chain length (ICL = CL ECL 1) of AP were turned to a water bath at 50 °C.9%. heated in boiling water for 10 min.06 0.13 Protein 0.1.03 Galactose 0.31 Monosaccharides The HPSEC system consisted of a pump (LC-20AD/LC-20AT. maltose (MW = 342. Arabinose 0.1 (SAS Institute. F3 with DP 25–36 and F4 with DP >36) accord.02 0. Cary. pullulanase (40 lL.12 0. I–II. the Statistical Analysis System software 8.5 82.02 M. Centrifugation after each washing step was at 3. It was then 2. (DP 2). 0.01 0. Barley b-amylase areas of the different regions were: I (DP 400–2650).04 0. 250 U/mL 0.04 0.

1) 14.4) 56.retro (°C) 67. as discussed below. gelatinisation intervals (Tc–To).retro. when gelatinised starches were stored at was indeed ‘intermediate’ in the sense that it behaved neither as 6 °C and rather small when compared to those of starches of other regular AM (it did not precipitate with n-BuOH reagent) nor as reg- botanical sources (barley.2) 68. / Carbohydrate Research 346 (2011) 2727–2735 2731 3. as percentage of the crystallinity of Nikita) of 92%. respectively.4 (0.2 Tc–To (°C) 14. temperature Treviso) and wheat (Zohra) flour. conclusion (Tc. Rye starch Wheat starch tween rye cultivars were also reported by Stoddard.9 (0.6) 64.8 (0.33. a lower setback atinisation temperatures than the wheat starch. Table 2 lists To.8 (0. respec- tively. The IM by Fredriksson et al. both isolated by the PronaseÒ- based isolation procedure was observed earlier. except for the starch from cultivar Tre- thalpy changes of the rye and wheat starches. similar viscosity behaviour. . respectively. S.7 (0. The wheat starch contained 20% B-granules.e.7 (0. 1). The starch from wheat cultivar Zohra had a relative crystallinity of 88%.2) 1.1 (0.1) described previously. IM and AP (Table 4). Nikita.2 15.retro and Tc.9 (0. DHretro is noticeably higher for the wheat ties (i. the three rye starches had a pasting temperature of approximately 72 °C and exhibited Table 2 represents the DSC gelatinisation temperatures and en.2) particle size of 26 lm (Fig. DSC gelatinisation and retrogradation properties istics.2) in Verwimp et al.retro. Nik. Properties of the non-granular starches and their starch tures of retrograded AP were observed between the investigated fractions starches. average onset (To. To. RVA viscograms of the starches (10% dm) isolated from rye ( .retro (°C) 56. Tp (°C) 53.1) 0.0) 55. cosities. enthalpy All starches showed a bimodal particle size distribution (Fig.6 (0. much among the starches. gelatinisation enthalpy changes (DH). WAXD pattern and relative crystallinity parenthesis.6 14.8) 48.2) a Averages of at least triplicate measurements. 100% cultivar Zohra than for the rye starches and is in agreement with and 93% were found for the starches from rye cultivars Avanti.2 Figure 2 shows RVA viscograms of the starches isolated from the rye and wheat flours and Table 3 summarizes their character- 3.5 (0.2 Differences in starch granule size distribution be. that is.7 (0.4 (0. which can be the starches may well be explained by differences in structure of explained by the lower lipid contents in the rye starches (Table 1).retro and 6000 100 90 5000 80 Temperature (°C ) 15 Avanti 70 Viscosity (cP) 4000 Volume percentage (%) Nikita 60 Treviso 3000 50 10 Zohra 40 2000 30 5 1000 20 10 0 0 0 0 5 10 15 20 25 30 35 40 45 0 10 20 30 40 50 60 70 80 90 100 Time (min) Granule size (µm) Figure 2. while those of the wheat starch had an average DHaml (J/g) 0.3) 2. 3. AM and AP. Avanti. Granule size distribution of the starches isolated from rye (Avanti.7 (0. (±78 °C). The differences in gelatinisation and pasting behaviour between served for the rye starches than for the wheat starch..8 (0.2) 50. Relative crystallini.6) 45. Somewhat lower DHaml values were ob.7 (0.3 (0.8 (0. Tp.33 A small enthalpy ular AP (part of the material eluted after the void volume in HPSEC. Under the experimental conditions.0 °C. profile).7 (0.6 (0.3 (0. Tc.1) 48. 2 and Table 3). Treviso) and wheat ( . These results are in line with average Tp. The wheat starch had a higher pasting temperature tures.1) 13. wheat and potato).2) 65.32 who exam- Avanti Nikita Treviso Zohra ined 50 rye cultivars and found B-granule content ranges To (°C) 49. Tc. Nikita. AM. Granule size distribution Table 2 Average gelatinisation onset (To).3 (0. which had lower breakdown and higher setback and end vis- the different rye samples showed similar gelatinisation tempera.2) 56.3) 3.2) between 21 and 39%.6 (0. Tp.4 (0.2) 0.4) 2. .1) particle sizes found for PronaseÒ-isolated rye and wheat starches Tc.8) 67.2) 52.0 (0.0) size of 30–31 lm.5) 45.4) 45. The melting enthalpy temperature ranges of retrograded Fractionation of the rye and wheat non-granular starches re- AP of rye and wheat starches are comparable to those obtained sulted in three fractions.6.0 (0. the rye starches had lower gel.9) 68.3 (0.4 (0. Figure 1.retro were observed.retro) temperatures of retrograded amylopectin and cultivars Avanti.2) in line with the value for PronaseÒ-isolated wheat starch described Tc (°C) 63.2 DHretro (J/g) 2.5 15. with standard deviations between 3. temperature range of retrograded AP pointed to a more uniform quality of the crystals.0) To.4) 62. RVA viscosity behaviour wheat starch than for rye starch.retro were ca. The volume percentage of B-granules was 26%.5. 1).9 (0. Nikita and Treviso. 45.3. A lower relative crystallinity for 3.1 (0. changes of the melting of amylose–lipid complexes (DHaml). In line with earlier results2. No differences in these tempera.retro). peak (Tp) and conclusion (Tc) temperatures.5 (0.33 ita and Treviso.6 (0.7 (0. The rye and wheat starches all showed an A-type polymorph with a small proportion of B-type polymorph. Fredriksson et al.8 (0.retro.retro).2.4 (0. .2) 56.7) 53.5 °C and 68.0 The A-type granules of the rye starches had an average particle DH (J/g) 13. DH did not differ and lower end viscosities than the rye starches (Fig. 21% and 17% for rye peak (Tp. These figures are enthalpy changes of retrograded amylopectin (DHretro) of the starches isolated from higher than the volume percentage of B-granules (14%) found for rye and wheat flour as measured by DSCa rye starches.4 (0. higher peak and breakdown viscosities. Gomand et al.retro and DHretro following storage of starches at 20 °C for 2 weeks. While no differences in To.4.2 (0.retro (°C) 45. V. The starches from viso. Zohra) flour ( .2) 13.

The AM fraction had higher extinctions at all 1000 0.2  104. Only for rye cultivar Tre- Extinction (620 nm) .625 0.a. 40.20 wavelengths (500–800 nm) (results not shown). Among the three rye samples.370 1. The chro. Treviso and finally Zohra.7 0. the IM of the rye and Figure 3.155 0.070 50 100 150 200 250 Nikita 0.105 0.4 6.2732 S. higher BV and higher 0 0. amylose tions at all wavelengths (500–800 nm) and BV of the IM decreased (AM). suggesting that the void .2 71. Nikita. 2. . followed by those of Nikita sidered to be AP.73  104.40 Avanti n. low BV and low kmax 78.00 cf.5 3. that is. 24. 24. and a broad fraction eluting after the void volume (2150) and Avanti (1850). .28  104 and of the AP fractions indicated that highly pure AP fractions were 1. RI (arbitrary units) .a. Zohra) and iodine binding ( . Nikita. the AM molecules from Tre- the void volume. .60 2500 Avanti Nikita Treviso Zohra 2000 Pasting temperature (°C) 71. MW markers (+) from left to right are 160. RI (arbitrary units) . .60 NG AM IM AP 2000 Yield (%) 0.565 0. Iodine binding of the non-granular 50 100 150 200 250 Time (min) starches and of their AM and AP fractions was nearly identical for the rye and wheat starches. Treviso) and wheat Extinction (620 nm) .2 1500 Nikita n.5 3. . For rye. / Carbohydrate Research 346 (2011) 2727–2735 Table 3 3500 0. Zohra).8  104. V.40 Peak viscosity (cP) 2650 2880 2900 3500 1500 Breakdown viscosity (cP) 790 930 690 1890 1000 0. but some differences in peak DP could be ob- matograms of the non-granular starches show a fraction eluting at served. 21.a. extinctions at all wavelengths (500–800 nm). in the order: Avanti. RI (arbitrary units) . The wheat starch AM fraction contained containing molecules of lower MW and considered to be AM as molecules with a lower peak DP (1750) than the rye starch AM demonstrated by their high iodine binding capacity.e. Extinc. Gomand et al. 3000 (Zohra) 2500 0.080 Zohra 0. .8 71. infra). 11. Figure 3 shows the SEC profiles of the non-granular rye and wheat starches and of their fractions. Avanti.385 1. 3000 Rye starch Wheat starch 0.40 1500 n.4  104.a.125 0. 23. The very low 4 Nikita.2  104.3 1000 0. viso had the highest peak DP (2400). broad knowledge.705 0. intermediate material (IM) and amylopectin (AP) and their corresponding blue value (BV) and kmax together with BV 3500 AM 0. were higher than those of the AP fraction. The yields of IM were 0. the non-granular 2000 0.60 Nikita 628 669 655 523 Treviso 631 671 655 538 2000 Zohra 629 654 646 538 0. 4.9 77.18  104. Avanti. IM and AP recovered were similar.20 Setback viscosity (cP) 1910 1990 2330 1750 500 End viscosity (cP) 4280 4430 5220 3830 0 0. Nikita. amylose (AM). distribution profiles were rather similar for the rye and wheat The iodine-binding values of the IM eluting at the void volume starches.2 70.2 72.9 73. 3000 viso a higher proportion of IM was obtained. Size-exclusion chromatography (SEC) (Sepharose CL-2B) elution profiles wheat starches showed different iodine binding properties.20 500 0 0.40 starting material and the three fractions had a different iodine 1500 binding behaviour.060 Time (min) Treviso 0.a. The existence of an IM fraction in rye starch was also ob- 50 100 150 200 250 served by Banks and Greenwood8 and Hew and Unrau. to the best of our The AM fractions of the different starches showed similar.00 Avanti 0.80 AP of AM.80 kmax (nm) Extinction (620 nm) .8 Table 4 presents BV and kmax. i. For each starch.9 72. obtained.680 0. RI (arbitrary units) .4 Zohra n. consisting of very high MW molecules and con.9 3.00 kmax than the AP fraction. which in its turn had higher extinctions at all wavelengths (500–800 nm). higher BV and 500 higher kmax than the IM fraction.00 50 100 150 200 250 Time (min) Table 4 Yield (%) of the starch fractions.0  10 .20 Treviso n. 3000 Avanti 629 656 652 538 2500 0.170 0.: not applicable 1000 0.080 3500 IM 0. Treviso.375 1. MW distributions. 22.7 500 BV 0 0.15 Time (min) Fractionation did not reveal significant differences among the rye starches and between the rye and wheat starches as the levels 3500 0.60 2500 in line with those reported earlier for rye and wheat starches. In contrast.80 RVA characteristics of the starches (10% dm) isolated from rye and wheat flour NG Extinction (620 nm) .390 1. Total carbohydrate ( . The overall fractions. of non-granular (NG) rye and wheat starches and their starch fractions. Treviso. intermediate material (IM) and amylopectin (AP).80 and kmax of non-granular (NG) starch from rye (Avanti. such profiles have not been reported earlier.

especially of those with DP 6–9. respectively) rye AP. respectively. lower than previously reported.8 cosities were observed for the wheat than for rye starches (Fig. S. however. The b-amylolysis limits of by HPSEC of the debranched AP b-limit dextrins.5 3. Table 5 Wheat starch tended to retrograde to a larger extent than rye b-Amylolysis limit. 15 and 20 and a larger proportion Some structural differences observed between the rye and of material with a DP of approximately 45. the higher level of BL chains in wheat AP While the HPAEC-PAD results yielded information on the chain (Fig. AP branch ylase and pullulanase and determining reducing groups released chain length distributions of the three rye samples were similar by the debranching enzymes.38 Vermeylen et al. informa. respectively. tinisation and pasting behaviour of the rye and wheat starches.5 0. / Carbohydrate Research 346 (2011) 2727–2735 2733 volume material in the IM contained molecules with branch chains Table 6 longer than those of AP.1 48. 1. that these val- Table 6 shows molar percentages of groups of unit chains in rye ues were determined by debranching b-limit dextrins with isoam- and wheat amylopectin determined by HPAEC–PAD. The latter is at variance with findings is more reliable for determination of the A:B chain ratio than for by Silverio and co-workers. Asaoka and co-workers49 reported that rice starches containing a higher proportion of long inner B-chains had higher gelatinisation temperatures. 12–13 and 8. Structural aspects in relation to physicochemical properties at DP 11. was obtained of the AP from rye and wheat starches.8 nearly identical for all rye and wheat AP (Table 5). The HPSEC method used in this study and showed a peak at DP 10. The wheat AP.7 2.9 2. Similar chain length distribu. has been reported. 2 BS:BL 2. bution of rye AP using HPSEC and HPAEC–PAD. Figure 4 shows the AP from the three rye samples were similar to each other (ca. was somewhat different from that of the samples were nearly identical (21–22.8 0.5 37. which is probably due to its lower level of chains with interior chain lengths (ICL). exterior chain lengths (ECL) and starches.8 0. however.5 and Table 3) might also be explained by the lower proportion of .15. respectively. That short chains Rye amylopectin Wheat amylopectin (DP <12) inhibit AP retrogradation while longer chains (DP 15–24) Avanti Nikita Treviso Zohra promote AP retrogradation. The interior chain length distribution of The average CL.7. An average CL of 20 The A:B chain ratios determined from the chromatograms were and 20–21 for rye and wheat AP.7 for wheat AP. The wheat AP had a higher Table 5 lists weight and molar percentages of A and B (BS and b-amylolysis limit than the rye AP.5 38.41–48 In addition. The average CL of the rye and wheat AP were in good agree. Structural aspects of amylopectin Table 5 lists the b-amylolysis limits and average CL. like wheat AM and AP molecules may explain the differences in gela- the rye AP. Nikita. however.0 suggested the presence of short branch chains.5 4. displayed a peak at DP 10.5 41.8. was already earlier described for b-Amylolysis limit (%) 48. 4). Gomand et al. In tion on the ICL distribution of the AP.8 0.9 starches of different botanical sources.3 49.5 0. The very F1 (DP 6–12) 57.34.17. Banks and Greenwood8 also found IM in Molar chain length distribution (%) of isoamylase debranched amylopectin from rye and wheat starches as determined by HPAEC-PAD rye and wheat starches containing AP-like molecules with some- what longer chain lengths than those of the AP fraction. The A:B chain Berry and co-workers5 found values of 21 and 23 for rye and wheat ratios (0.36 however. It should be noted.37 who studied the chain length distri. Gidley (Zohra) and molar chain ratios of A:B and short B chains to long B chains (BS:BL) of and Bulpin50 described that at least 10 glucose units are needed for their debranched b-limit dextrins double helix formation of maltooligosaccharides. and Lineback36 found an A:B chain ratio of 1. BL) chains as well as the molar ratios of A:B chains and of BS:BL ferences between wheat and rye AP. but of higher MW than those of the AM fraction. the mass and molar based chromatograms of the debranched b- 48–49%) but lower than those reported by Banks and Greenwood8 limit dextrins of the rye and wheat starch AP. tion temperatures found for the wheat than for the rye starches. suggesting some structural dif.5 4. the measurement of reducing power. The b-amylolysis limit of the chains.0 low iodine binding of the AP fractions confirmed their purity and F2 (DP13–24) 37. No differences negatively and positively.8) were.5 4. ECL and ICL knowledge.8 2. average chain lengths (CL).7 53. The AP from the different rye samples has similar distribu- wheat AP was in line with earlier reported values. (58%) and Hew and Unrau15 (57–61%). ature. respectively. The wheat AP had a somewhat higher average CL (23) (regions I and II) and a lower proportion of shorter B chains (region and ECL (14) and a somewhat lower ICL (7) than the rye amylopec. BS and BL chains.5 F4 (DP >36) 0. Lii AP. of rye (Avanti. ECL and ICL of the AP from the different rye the wheat AP.8 for rye AP and age CL for rye AP (26) than for wheat AP (17–20). Avanti Nikita Treviso Zohra cules. ICL (DP) 8 8 8 7 The higher pasting temperature and peak and breakdown vis- A:B 0. which. F3 (DP 25–36) 4. The wheat AP contained a larger proportion of long B chains (Table 4).5 54.5 56.51. tion profiles for wheat AP with a peak at DP 10–11 were reported The higher gelatinisation temperatures found for the wheat by Koizumi and Fukuda.2–1. has not been reported before for rye. while the latter found distribution patterns which showed peaks at DP 12. 4 and Table 5) might also contribute to the higher gelatinisa- length distribution of the shorter chains of AP (DP <60). to the best of our this respect. The IM Rye amylopectin Wheat amylopectin eluting after the void volume appeared to contain AM-like mole.5 57. The wheat AP had a lower level earlier for starches from different botanical sources that the distri- of chains with DP 6–12. AP than for the rye AP. V. The former authors found chain length distributions with peak maxima 3. 18 and 47. with gelatinisation temper- were found in the distribution of chains with DP >24.5 0.8. Lii and Lineback. found a higher aver. The ratio of BS:BL chains was also somewhat lower for the wheat tin.40 proportion of chains with DP 6–12 and the higher proportion of The chain length distribution profiles of the rye and wheat AP chains with DP 13–24 in the wheat AP (Table 6).48. and a bution of AP unit chains with DP 6–12 and DP 13–24 correlates higher level of chains with DP 13–24 than rye AP. Treviso) and wheat amylopectins DP 6–12 and higher level of chains with DP 13–24 (Table 6).39 and Wickramasinghe starch than for the rye starches (Table 2) might be due to the lower et al.35 tions of A. no relations CL (DP) 22 21 22 23 existed between structural properties and enthalpic temperatures ECL (DP) 13 12 13 14 of retrograded AP as the latter did not notably differ. It was reported showed some differences (Table 6).52 Logically. ment with those found in earlier studies.

267–272. G. 1993. positively with the level of AP unit chains with DP 6–12 and DP 6. Preiss. Ball.. had a somewhat higher b-amylolysis limit. High-performance size exclusion chromatography (HPSEC) (Zorbax PSM 60S columns) elution profiles of debranched b-limit dextrins from rye (Avanti. retrogradation and pasting 30 behaviour between the rye and wheat starches. B. 4. 20 Acknowledgements 10 0 We thank Hilde Van den Broeck. MW markers (+) from left to right are 11. average CL and ECL and a somewhat lower ICL than the rye AP. average CL. 19.. A. K. 3rd ed. Colonna. Be- Time (min) sides. H. Gernat.. Cereal Sci. 3) might explain the differences in set- 50 back and end viscosities of the rye and wheat starches (Fig. For starches from different botan. the rye and wheat starches were fractionated Relative moles . 43. Carbohydr. Starch/Stärke 1993.2734 S. S. Conclusions 50 Nikita Starches were isolated from three rye flour samples and one RI (arbitrary units) . E.. however. 10 12 14 16 18 20 22 The wheat AP. Buléon. V.53. J. Res. 415–427. pasting temperature correlated negatively and 5. S. P. Cereal Chem. However. Qin. no significant correlations between AP chain 11. length distribution and peak and breakdown viscosity of starch 12. P. 1971.. Cereal Chem. 13–24. A. Richter. F. 85–90. The rye starches differed from the Time (min) wheat starch in showing a somewhat higher relative crystallinity... D. Zobel. RI (arbitrary units) .. 2003. E. containing molecules with long branch chains. Marrant. glucose. Greenwood.18  10 . 1998. Gomand et al..43. A. T. A. Some differences in AM 30 peak DP were found among the rye samples and between the rye 20 and wheat samples.. Lim. lower peak and Treviso breakdown viscosities and higher setback and end viscosities. Hizukuri. 10. The differences in AM and AP structure may ex- Relative moles . 42. K. 1993. 50 and a lower tendency to retrograde. 86.54 whereas. 246. Mua and Jackson56 30 also reported a positive correlation between AM DP and setback 20 and final viscosity of maize starch. Barbara Vangeneugden and 10 12 14 16 18 20 22 Luc Van Den Ende for technical assistance... White. 420–425.. Verwimp. Myers.73  10 . K. Gelatinisation and AP retrogradation behaviour of rye and 10 12 14 16 18 20 22 wheat starches did not differ. Guan. C.. and Relative moles . P. . These re- 50 sults demonstrate that the structure of the wheat AP differs from RI (arbitrary units) . 45. 2 RI (arbitrary units) . in other studies. J. Colonna. maltopentaose. were found between the content of AP short chains (DP 6–12) 8.. Carbohydr. 40. In the second part. ical sources. Banks. indicating that different rye AP had similar structures. C. 521–525.. Bertoft. M..-W. Cell 1996. Berry. C.55 The different peak DPs observed for the rye and 13. D.U. Time (min) Leuven. 338. J. 40 plain the differences in gelatinisation. Jane. wheat AP had a lower proportion of chains with DP 6–12 and Zohra a higher proportion of chains with DP 13–24 than rye AP.. J. Starch/Stärke 13–24 in the wheat AP (Table 6). might also I II III IV V VIVII 0 contribute to the higher setback and end viscosities found for this 10 12 14 16 18 20 22 cereal (Fig. New Insights on Starch Structure and Properties. 75. 682–683. 40 their physicochemical and structural properties were analysed. 1992. the higher propor- tion of IM in rye cultivar Treviso than in the other rye cultivars (Ta- 10 ble 4). Thompson. B. H. M. 40 into their AM. Delcour. that of the rye AP. Keeling. Rye AP showed some minor differences in b- amylolysis limit. 887–896. 394–398. Radosta. J. W.53–55 In some studies. 1... wheat flour sample by a PronaseÒ-based isolation procedure. Buléon. lower gelatinisation and pasting temperatures. Res. H. 2 and Table 3). Starch/Stärke 1967. Lit- 30 tle if any differences in physicochemical properties between the 20 rye samples of different origin were observed.-T. S. Wang. B.. maltoheptaose. Vandeputte.. negative correlations 7. L. Z.. 1991. 70. the rye 10 cultivar Treviso had a somewhat lower breakdown and higher set- back and end viscosities than the starches from the other rye cul- 0 tivars. Poutanen. References Nikita. 9th International Cereal and Bread Congress. L. A. 48. 44–50. Furthermore. P. 39. James. S.. S. Figure 4. Kettlitz. were found. and Table 3). 0. Takeda..2  104.. D’Appolonia. pp chains with DP 6-12 and the higher proportion of chains with DP 25–42. Mouille. 331–339. Y. Y. This study is part of the Methusalem programme ‘Food for the Future’ at the K.59  10 . / Carbohydrate Research 346 (2011) 2727–2735 Avanti wheat AM molecules (Fig. Cereal Chem. F. 3. P. 4 4 4 1. Mass-basis ( ) and molar-basis ( ) chromatograms. Cereal Foods World 1997. Tomooka. Manelius.. G. In: Cereal Chemistry and Technology: A Long Past and A Bright Future— Proceedings. Time (min) 4. Klucinec. 4.. respectively. 349–352. maltose and 2. Yoon. IM and AP components. P. T. Starches containing AM molecules with a higher DP Relative moles . Schierbaum. Starch/Stärke 1988. 40 exhibited higher setback and end viscosities. Pollak. Treviso) and wheat (Zohra) amylopectin. 9. 2004. J. and the peak and breakdown viscosities of starch.. R. Gilles. ECL and ICL and had nearly identical 10 chain length distributions and similar interior chain length distri- 0 butions. 611–617.

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