Microscopic Study of Starch Gelatinization under High Hydrostatic

Pressure
J. P. Douzal s,

P. A. Marechal ,

J. C. Coqui l l e,

and P. Gervai s*
,
Laboratoi re de Geni e des Procedes Al i mentai res et Bi otechnol ogi ques, ENSBANA, 1 Espl anade Erasme,
21000 Di jon, France, and Laboratoi re de Geni e des Agro-equi pements et des Procedes, ENESAD,
Bd. O. de Serres, 21800 Queti gny, France
Starch gel ati ni zati on corresponds to a mel ti ng phase transi ti on i n aqueous medi um. Such a
transi ti on i nvol ves i mportant mass transfer of water. Usi ng a hi gh-pressure bomb i ncl udi ng opti cal
ports, the vol ume vari ati on of starch granul es i n suspensi on was rel ated to gel ati ni zati on duri ng a
hi gh-pressure treatment up to 420 MPa. Mi croscopi c observati ons of wheat and potato starch
granul es were compared wi th macroscopi c measurements of compressi bi l i ty up to 600 MPa and
gel ati ni zati on i ntensi ty usi ng di fferenti al scanni ng cal ori metry on treated suspensi ons. Wheat starch
gel ati ni zati on started bel ow 300 MPa and was compl etel y achi eved at 600 MPa. Potato starch was
not al tered under 600 MPa. The behavi or of the vol ume vari ati on of starch granul es under pressure
compared wi th starch suspensi ons compressi bi l i ty coul d be expl ai ned by si mul taneous compressi on
and hydrati on mechani sms.
Keywords: Starch gelatinization; high hydrostatic pressure; imageanalysis
I NTRODUCTI ON
Starch gel ati ni zati on consi sts of a bi opol ymer mel ti ng
i n an aqueous medi um. When a water-starch suspen-
si on i s heated, a phase transi ti on i s observed for starch
between 60 and 70 C. Opti cal properti es of starch
granul es, such as l i ght pol ari zati on or i odi ne col orati on,
are changed.
Granul e swel l i ng i ncreases wi th temperature and
becomes i rreversi bl e when gel ati ni zati on occurs. The
swel l i ng corresponds to a mass transfer of bul k water
i n the suspensi on to water l i nked wi th starch compo-
nents (amyl ose and amyl opecti n). General l y, granul e
structure i s di spersed when heat treatment reaches a
certai n l evel , and the sol ubi l i zati on of amyl ose chai ns
i s responsi bl e for an i ncrease i n vi scosi ty.
Starch gel ati ni zati on i s an endothermi c transi ti on
whi ch i s wel l i denti fi ed wi th di fferenti al scanni ng
cal ori metry (DSC). Thi s method al l ows the character-
i zati on of mel ti ng parameters, i .e., enthal py of gel ati -
ni zati on (H
f
) and temperature of mel ti ng (endothermi c
peak temperature).
Hi gh-pressure technol ogy has been known si nce the
begi nni ng of the 20th century (Bri dgman, 1914), but
appl i cati ons i n the food i ndustry have onl y been devel -
oped i n the past 20 years, parti cul arl y i n Japan and
Europe (Suzuki and Tani gushi , 1972; Weber and Dri ck-
amer, 1983; Gekko and Fukami zu, 1991a,b; Dumay et
al ., 1994).
Si nce 1980, several papers have i ndi cated that hi gh-
pressure gel ati ni zati on of starch i s possi bl e wi th a heat
treatment before compressi on (Muhr and Bl anshard,
1981; Hayashi , 1992; Kudl a and Tomasi k, 1992; Hi bi
et al ., 1993). Some research i nvol ved hi gh-pressure
di fferenti al thermal anal ysi s (HPDTA), whi ch al l owed
a si mul taneous appl i cati on of pressure and heati ng
(Muhr et al ., 1982). These authors have cal cul ated the
vol ume vari ati on of starch duri ng gel ati ni zati on under
pressure by usi ng Cl apeyrons equati on (1), whi ch i s
val i d for any phase transi ti on at equi l i bri um:
T i s the absol ute mel ti ng temperature, P i s the pressure,
and G, V, and H are the speci fi c Gi bbs free energy,
vol ume, and enthal py changes, respecti vel y. V i s the
vol ume change of 1 g of starch crystal l i tes di ssol ved i n
an i nfi ni te reservoi r of the water-starch mi xture. H,
dP/dT, and T
m
measurements permi t one to cal cul ate
the correspondi ng V. Resul ts from these cal cul ati ons
i ndi cated a reducti on of starch vol ume of 0.5 mm
3
/g of
crystal l i tes at 400 MPa and an i ncrease i n vol ume of
about 1 mm
3
/g under atmospheri c condi ti ons.
Recent research on starch gel ati ni zati on under pres-
sure showed a better enzymati c di gesti bi l i ty of treated
starch (Hayashi and Hayashi da, 1989). Pressure coul d
al so del ay starch gel retrogradati on.
The ai m of thi s paper was to compare mass transfer
observati ons from mi croscopi c study of starch granul es
under hi gh pressure wi th macroscopi c measurements
of energy or vol ume vari ati on of starch suspensi ons.
Mi croscopi c observati ons of starch granul es were per-
formed by an ori gi nal vi sual i zati on system worki ng
under pressure. These two scal es of observati on woul d
al l ow one to understand the mechani sm of starch
gel ati ni zati on under pressure and especi al l y the con-
tri buti on of water-starch i nteracti ons.
MATERI ALS AND METHODS
Starch. Wheat starch (ref E123359, Merck, France) con-
si sted of 23% amyl ose and 75% amyl opecti n (w/w). Moi sture
content was measured after 24 h of dryi ng at 105 C and was
16.4 ( 0.5% on a dry matter basi s. Speci fi c densi ty measure-
ments usi ng the pi cnometri c method gave a val ue of 1.29 (
0.1 g cm
-3
.
Potato starch (ref 21146290, Prol abo, France) consi sted of
26% amyl ose and 73% amyl opecti n (w/w). Moi sture content
* Author to whom correspondence shoul d be ad-
dressed (fax 33 80 39 66 11; e-mai l gervai s@
u-bourgogne.fr).

ENSBANA.

ENESAD.
T
P
|
G)0
) T
V
H
(1)
1403 J. Agric. Food Chem. 1996, 44, 14031408
S0021-8561(95)00239-1 CCC: $12.00 1996 American Chemical Society
was 14.8 ( 0.5% on a dry matter (DM) basi s. Speci fi c densi ty
measured i n the same condi ti ons was 1.31 ( 0.1 g cm
-3
. For
each experi ment, water-starch suspensi ons were prepared 1
h before pressure treatment and were conti nuousl y sti rred at
20 C.
Mi croscopi c observati ons were dependent on the l arge scal e
of starch granul e di ameter. Tabl e 1 i ndi cates mean di ameters,
extreme di ameters, and di stri buti on mode for 768 wheat
granul es and 652 potato granul es col ored wi th i odi ne.
High-PressureVisualization Cell. Mi croscopi c observa-
ti ons were obtai ned by a uni que hi gh-pressure cel l (25 L, 700
MPa) manufactured by LI MHP, CNRS, Vi l l etaneuse, France.
The copper beryl l i um body cel l i ncl uded opti cal ports (sapphi re
wi ndows) of 10 ( 0.1 mm di ameter, 5 mm thi ck for the l ower
one, 10 mm thi ck for the upper one, through whi ch l i ght can
pass.
The hi gh-pressure chamber (0.8 mm thi ck) was si tuated
between the two sapphi res and connected to a hi gh-pressure
system. To prevent l eaks, di fferent ki nds of gol d joi nts and
gaskets were used.
Starch suspensi ons were 0.1%starch content (starch wei ght/
suspensi on wei ght on a dry matter basi s) and prepared wi th
di sti l l ed water at room temperature. The hi gh densi ty of the
starch granul es prevented them from movi ng i n the hi gh-
pressure cel l duri ng the ti me of pressure appl i cati on.
Microscopy and Image Analysis System. The hi gh-
pressure cel l was pl aced on an i nverted l i ght mi croscope usi ng
an objecti ve l ens 20 (Nachet, France). I mages were observed
di rectl y through a bi nocul ar and recorded vi a a charge coupl ed
devi ce (CCD) camera. Thi s system al l owed i mage anal ysi s
usi ng Vi si l og Software (Noesi s, France). Each i mage consi sted
of a 256 256 pi xel matri x of 256 gray l evel s and contai ned
about 30 granul es. Granul es were i ndi vi dual l y anal yzed to
fi nd thei r projected area (S) i n compari son wi th gl ass bal l s of
10 m di ameter. Starch granul es were assumed to be spheri -
cal .
Then, vol ume (V) was cal cul ated usi ng the fol l owi ng equa-
ti on:
Speci al care was taken wi th focus and l i ghtness adjustment.
I mage threshol di ng condi ti ons were kept constant duri ng al l
of the experi mentati on.
The error i n cal cul ati on of di ameter and vol ume di d not
exceed 4%. Furthermore, starch granul es were i odi ne col ored
because of the excel l ent contrast needed for i mage anal ysi s.
Starch granul e vi sual i zati on was achi eved under pressure
duri ng two cycl es of pressuri zati on at room temperature.
I mage anal ysi s al l owed the fol l owi ng of i ndi vi dual granul es
and thei r speci fi c change every 100 MPa.
High-Pressure System for Microscopic Measure-
ments. As shown by Fi gure 2, pressure was generated wi th
a 400 MPa hydropneumati c pi ston pump (Haskel , 903 C, Great
Bri tai n). Di sti l l ed water was used as compressi on fl ui d.
Pressure was measured wi th a 700 MPa pressure gauge (G515/
7000, Sedeme, France) wi th a preci si on of 0.5%. The pressure
was transmi tted to the vi sual i zati on cel l vi a
1
/4 i n. tubi ng. Thi s
hi gh-pressure system i ncl uded val ves, fi tti ng, and tubi ng
desi gned for hi gh-pressure work. The compressi on rate was
about 5 MPa s
-1
and was the same for each experi ment. Two
cycl es of pressuri zati on were carri ed out at the same pressure
l evel .
High-Pressure Systemfor Compressibility Measure-
ments. Pressure was generated wi th a 700 MPa manual
screw pi ston pump of 3 mL (Nova Swi ss, Swi tzerl and).
Suspensi ons contai ned 16% starch (DM basi s) and were
compressed i nto the body of the pump. Vol ume changes (V)
were measured through the vari ati on of the i ni ti al posi ti on of
the screw wi th the pressure vari ati on. Pressure ranges were
about 10 MPa per poi nt of measure. Compressi on and rel ease
were control l ed at a rate of 50 MPa s
-1
but can be sl owed down
i f necessary. Two cycl es of pressuri zati on were achi eved upon
the same suspensi on.
The parameter compressi bi l i ty, whi ch i s usual l y empl oyed
when a pure l i qui d i s consi dered, i s not exactl y appropri ate
for thi s work. The i ni ti al bi phasi c suspensi on was transformed
to a di spersi on duri ng the hi gh-pressure treatment. Then,
macroscopi c compressi bi l i ty of l i qui ds i s gi ven by the equati on:
where t i s the macroscopi c compressi bi l i ty of the suspensi on
i n bar
-1
, V i s the vol ume change of the suspensi on i n
mi l l i l i ters, V i s the i ni ti al vol ume i n mi l l i l i ters, and P i s the
pressure vari ati on i n bar. Preci si on of the compressi bi l i ty
measurement was about 1%.
The i ni ti al vol ume was determi ned wi th pure water usi ng
Tai ts equati on (Hayward, 1967) and gi ven by
where K0 i s the bul k modul us at zero pressure i n bars and m
the sl ope of the bul k modul us pressure curve as descri bed by
Hayward (1967). P and V are gi ven i n bars and mi l l i l i ters,
respecti vel y. The val ues of coeffi ci ents m) 3.306 and K0 )
22421 were esti mated from pure water compressi bi l i ty mea-
surements. I ni ti al vol ume V was found to be equal to 4.78 (
0.01 mL.
I ni ti al vol ume determi nati on was dependent on a compl ete
fi tti ng of the hi gh-pressure system. So a pri mary vacuum was
appl i ed.
Energetical Measurements after a Pressure Treat-
ment. Usi ng the hi gh-pressure system descri bed for com-
pressi bi l i ty measurements, starch suspensi ons were com-
pressed from 100 to 600 MPa. The enthal py of gel ati ni zati on
(Hf) and the temperature of maxi mum peak (Tm) were
subsequentl y determi ned usi ng di fferenti al scanni ng cal ori m-
etry (DSC) wi th three repeti ti ons. The DSC apparatus was a
Perki n-El mer DSC2 wi th a temperature preci si on measure-
ment of 0.1 K and 0.5 J g
-1
dry matter for enthal py of
transi ti on, whi ch was manual l y determi ned.
RESULTS AND DI SCUSSI ON
Microscopic Observations of Starch Granule
Gelatinization under High Pressure. Fi gure 1a
represents the i odi ne col ored wheat starch granul es i n
suspensi on wi th water at atmospheri c pressure. Fi gure
1b represents the same granul es at 420 MPa. Some
wheat granul es l ost thei r i odi ne col orati on, and si gni fi -
cant swel l i ng was observed above 300 MPa. No noti ce-
abl e effect on the di ameter was shown: gel ati ni zati on
seemed to affect smal l or l arge granul es equal l y.
The evol uti on of the vol ume of about 90 wheat
granul es was represented on compressi on and rel ease
i n Fi gure 3. The maxi mum pressure appl i ed was 420
MPa. Two popul ati ons were i denti fi ed, wi th regard to
thei r subsequent behavi or, and the di scri mi nati on was
observed above 300 MPa on compressi on. About 25%
of wheat granul es were swol l en wi th a si mul taneous
i odi ne di scol orati on, whi ch i ndi cated starch mel ti ng.
Thi s i ncrease i n granul e vol ume was parti cul arl y
rel evant between 300 MPa on compressi on and 300 MPa
on rel ease. At the end of the rel ease, mel ted wheat
granul e swel l i ng reached 78% for the mean. On the
Table 1. Diameter Distribution for Wheat and Potato
Starch Observed by Microscopy in Reference to Glass
Balls of 10 mDiameter
a
starch mean di ameter (m) extremes (m)
wheat
1
b
10 3-17
2
b
29 18-58
potato 37.5 10-110
a
Preci si on of the di ameter measurement was about 5%.
b
Di s-
tri buti on was bi modal for wheats 1 and 2 and uni modal for potato.
V ) 4S
3/2
/3 (2)

t
) -V/V(P) (3)
V/V ) P/[P(m) + K
0
] (4)
1404 J. Agric. Food Chem., Vol. 44, No. 6, 1996 Douzals et al.
other hand, undamaged granul es were onl y modi fi ed at
the end of the rel ease when a sl i ght swel l i ng of 25%was
observed wi thout i odi ne di scol orati on.
The same granul es were submi tted to another pres-
sure cycl e at the same l evel as shown i n Fi gure 4 i n
whi ch the evol uti on of wheat granul e vol ume i s pl otted
versus pressure duri ng the compressi on and rel ease
phases. Unl i ke previ ous resul ts, the vol ume of wheat
starch granul es was found to decrease duri ng the
compressi on phase and i ncrease duri ng the rel ease,
showi ng a reversi bl e behavi or under pressure. No
further swel l i ng or i odi ne di scol orati on occurred duri ng
the second cycl e.
Change i n the vol ume of potato starch under pressure
i s shown i n Fi gure 5 for the fi rst and second cycl es.
Maxi mum pressure was 300 MPa.
Fi rst compressi on i nduced an i rreversi bl e swel l i ng of
15% observed at the end of the rel ease of the fi rst cycl e,
but no di scol orati on occurred. A second compressi on at
the same l evel i nvol ved a reducti on of granul e vol ume
under pressure. No further modi fi cati ons were observed
i n terms of swel l i ng or i odi ne di scol orati on.
These pri mary resul ts showed that wheat and potato
starch granul es di d not reduce thei r vol ume when
pressure i ncreased. Moreover, a si gni fi cant number of
wheat starch granul es swel l ed and di scol ored duri ng the
compressi on phase and l ooked gel ati ni zed. Potato and
undamaged wheat granul es were onl y sl i ghtl y swol l en
at the end of the fi rst cycl e. Those granul es remai ned
i odi ne col ored, so onl y hydrati on can be suggested to
expl ai n such an i ncrease i n granul es vol ume.
Whatever modi fi cati ons were i nduced by pressure, a
second pressuri zati on gave reversi bl e resul ts for wheat
as wel l as for potato granul es.
Calorimetric Analysisof Water-Starch Suspen-
sions Treated by High Pressure. Macroscopi c mea-
surements of energy were carri ed out on starch suspen-
si ons to confi rm mi croscopi c resul ts. DSC gave a
quanti tati ve i ndi cati on of starch gel ati ni zati on on sus-
pensi ons previ ousl y treated under pressure.
DSC resul ts were provi ded by thermograms (Fi gure
6), on whi ch mel ti ng enthal py (H
f
) was gi ven versus
temperature for wheat starch. Tabl e 2 i ndi cates the
mel ti ng enthal py and the percentage of mel ted mass
versus pressure referri ng to i ni ti al sampl e mass of
wheat starch. DSC resul ts at atmospheri c pressure
were accordi ng to previ ous work (El i asson, 1980; Lund,
1984) whi ch i ndi cated H
f
of 13.5 and 13.2 J g
-1
of
wheat starch DM, respecti vel y.
Potato starch gave no rel evant modi fi cati ons of gel a-
ti ni zati on enthal py, and resul ts are not presented there.
As shown i n Fi gure 6, a si gni fi cant decrease i n peak
area was observed after a 300 MPa treatment, and
wheat starch thermograms i ndi cated no more mel ti ng
enthal py after a 600 MPa treatment. I t can be con-
cl uded that, i n thi s case, starch had al ready mel ted
under pressure.
Hence wheat starch gel ati ni zati on can occur between
300 and 500 MPa wi th, respecti vel y, 15-88% of mel ted
starch mass i n reference to i ni ti al sampl e mass. I n
compari son wi th a hi gh-pressure treatment, starch
gel ati ni zati on under atmospheri c condi ti ons i s com-
pl etel y achi eved at about the mel ti ng temperature ((10
C). A hi gh-pressure treatment woul d al l ow graduated
l evel s of gel ati ni zati on.
Evolution of the Compressibility of a Water
Starch Suspension under Pressure. Wheat and
potato starch suspensi ons were compressed up to 600
MPa usi ng a manual hi gh-pressure pump. Usi ng the
conveni ent representati on of a pure l i qui d compress-
i bi l i ty gi ven by eq 3, starch suspensi on compressi bi l i ty
was cal cul ated versus pressure.
The evol uti on of a wheat starch suspensi on duri ng
the compressi on and rel ease phases i s represented i n
Fi gure 7. Duri ng the compressi on bel ow 300 MPa, the
compressi bi l i ty of a starch suspensi on was cl ose to that
of pure water. Over 300 MPa, the reducti on of the
vol ume was hi gher for the starch suspensi on than for
pure water at the same pressure. At 600 MPa, vol ume
reducti on was 14.1% for pure water and 15.7% for the
starch suspensi on. Duri ng the rel ease, as shown i n
Fi gure 7, the starch suspensi on compressi bi l i ty was
al ways hi gher than that of water. Furthermore, the
starch suspensi on was of hi gher compressi bi l i ty than
water when measured duri ng the compressi on phase for
the same pressure val ue. A vol ume reducti on remai ned
si gni fi cant after return to atmospheri c pressure. When
starch suspensi ons were submi tted to another pressure
Figure 1. (a, top) Suspensi on of wheat starch granul es i n
water at room temperature. Starch granul es have been i odi ne
col ored. (b, bottom) Suspensi on of wheat starch granul es at
420 MPa. Gel ati ni zed granul es have l ost thei r i odi ne col ora-
ti on. Undamaged granul es are sti l l i odi ne col ored.
Starch Gelatinization under High Hydrostatic Pressure J. Agric. Food Chem., Vol. 44, No. 6, 1996 1405
cycl e at the same l evel , the compressi bi l i ty of the starch
suspensi ons was found to be equal duri ng the compres-
si on and rel ease phases.
Potato and wheat starchs gave qui te si mi l ar resul ts
except for the ampl i tude of the l ags whi ch was l ower
for potato. Therefore, onl y wheat starch resul ts are
represented.
Mi croscopi c resul ts showed that wheat starch gel a-
ti ni zati on under pressure was fol l owed by si gni fi cant
granul e swel l i ng and di scol ori ng. Hydrati on can be
suggested for undamaged wheat and potato granul es
that swel l ed. Compressi bi l i ty measurements i ndi cated
a reducti on of the suspensi on vol ume whi l e wheat starch
was mel ti ng.
Thi s apparentl y paradoxi cal behavi or i ndi cated that
water-starch i nteracti ons under pressure were onl y
possi bl e wi th a reducti on of the total vol ume, accordi ng
to Le Chatel i ers pri nci pl e. A schemati c representati on
of wheat starch granul e behavi or under pressure i s
gi ven i n Fi gure 8. Duri ng the compressi on phase, the
starch granul e vol ume di d not decrease as predi cted by
starch compressi bi l i ty under pressure (Kudl a and To-
Figure 2. Hi gh-pressure ci rcui t, vi sual i zati on cel l , and i mage anal ysi s equi pment.
Figure3. Vol ume i ncrease i n wheat starch granul es duri ng
the compressi on and rel ease phases for mel ted (30) and
undamaged (60) granul es i n reference to i ni ti al vol ume. Bars
represent the confi dence i nterval of the mean (95% l evel ).
Figure4. Vol ume evol uti on of mel ted wheat granul es duri ng
the compressi on and rel ease phases for two cycl es of pres-
suri zati on i n reference to i ni ti al vol ume. Bars represent the
confi dence i nterval of the mean (95% l evel ). B, begi nni ng of
the cycl e; E, end of the cycl e.
1406 J. Agric. Food Chem., Vol. 44, No. 6, 1996 Douzals et al.
masi k, 1983). So, i t coul d be suggested that hydrati on
occurred i n the case of damaged wheat granul es.
Granul e hydrati on woul d al l ow preservati on of the
i ni ti al granul e vol ume and so woul d counteract the
compressi on effect. The macroscopi c consequence of
starch hydrati on was a decrease i n the bul k suspensi on
vol ume. Such a behavi or was veri fi ed for undamaged
wheat and potato granul es.
As shown i n Fi gure 8, some wheat granul es were
swol l en and di scol ored above 300 MPa, whi l e the
suspensi on vol ume was more restri cted than that of
pure water. Thi s di scol orati on was confi rmed by DSC
measurements and was found to correspond to starch
granul e gel ati ni zati on. Thi s phase transi ti on i nvol ved
a massi ve water entry i nto starch granul es and the
creati on of hydrogen bonds between water and starch
enhanced by the hi gh-pressure l evel . Thi s granul e
swel l i ng was accompani ed by a reducti on of the bul k
suspensi on vol ume.
To expl ai n the previ ous observati ons, the water
mol ecul es l i nked wi th starch must then occupy a
smal l er vol ume than the mol ecul es i n pure water. Such
an expl anati on val i dates the pri nci pl e of Le Chatel i er
and appears to be consi stent wi th previ ous works
Figure5. Vol ume evol uti on of 60 potato granul es duri ng the
compressi on and rel ease phases for two cycl es of pressuri zati on
i n reference to i ni ti al vol ume. Bars represent the confi dence
i nterval of the mean (95% l evel ). B, begi nni ng of the cycl e; E,
end of the cycl e.
Figure 6. DSC thermograms of wheat starch suspensi ons
(16% w/w DM basi s) after di fferent l evel s of pressuri zati on.
Table 2. Evolution of the Enthalpy of Gelatinization
(Hf) and of the Gelatinized Mass (in Reference to Initial
Mass of Dry Matter) with Pressure Increase for Wheat
Starch-Water Suspensions
a
pressure (MPa) Hf (J g
-1
) gel ati ni zed mass (%)
0 17.9 0
100 17.8 0
200 17.9 0
300 15.2 15
400 12 33
500 2 88
600 0 100
a
16% w/w DM basi s. The preci si on i n Hf measurement i s (
0.5 J g
-1
of DM and (2.8% for starch gel ati ni zed mass.
Figure 7. Evol uti on of the compressi bi l i ty (t) of a wheat
starch suspensi on (16%starch content w/w DM basi s) and pure
water duri ng a cycl e of pressuri sati on. B, begi nni ng of the
cycl e; E, end of the cycl e.
Figure8. Schemati c representati on of wheat starch granul e
behavi or i n suspensi on wi th water duri ng a 400 MPa treat-
ment.
Starch Gelatinization under High Hydrostatic Pressure J. Agric. Food Chem., Vol. 44, No. 6, 1996 1407
i mpl i cati ng hydrogen bonds under pressure (Suzuki and
Tani gushi , 1972; Gekko and Fukami zu, 1991a,b).
Concerni ng potato starch, our resul ts were i n agree-
ment wi th previ ous work i ndi cati ng a total gel ati ni za-
ti on of potato starch at onl y 800 MPa at room temper-
ature (Kudl a and Tomasi k, 1992). These authors
suggested that the parti cul ar behavi or of potato starch
under pressure was rel ated to speci fi c crystal l i ne con-
formati on.
CONCLUSI ON
Compari son of mi croscopi c and macroscopi c measure-
ments al l owed to more preci se understandi ng of starch
gel ati ni zati on under pressure. Mi croscopi c observati ons
showed that wheat starch gel ati ni zati on began above a
pressure of 300 MPa wi thout previ ous heati ng. Thi s
phenomenon occurred duri ng the compressi on phase for
wheat starch granul es as confi rmed by DSC resul ts. At
420 MPa, 33% of the starch mass had mel ted. From a
macroscopi c poi nt of vi ew, pressure i nduced wheat
starch hydrati on and a compl ete gel ati ni zati on at 600
MPa. These two phenomena i nvol ved a reducti on of the
bul k suspensi on vol ume as wel l as an i ncrease i n
granul e vol ume.
Hi gh pressure enhanced i rreversi bl e transformati ons
duri ng the fi rst pressuri zati on cycl e. A second cycl e at
the same pressure l evel gave no further modi fi cati ons.
As shown wi th cal ori metri c anal ysi s, wheat starch
gel ati ni zati on was found to be graduated as a functi on
of the pressure l evel . Thi s behavi or, whi ch di d not occur
for a thermal treatment, coul d have technol ogi cal ap-
pl i cati ons.
I ndeed, such graduated gel ati ni zati on al l ows preser-
vati on of starch granul e i ntegri ty and so woul d prevent
amyl ose sol ubi l i zati on, whi ch i s responsi bl e for l arge
vari ati ons of vi scosi ty.
I t has been shown that starch gel ati ni zati on under
pressure l ed to speci fi c water-starch l i nkages. Further
works woul d al l ow veri fi cati on i f such a speci fi c struc-
ture woul d correspond to parti cul ar functi onal proper-
ti es, such as rheol ogi cal properti es and retrogradati on
mechani sms.
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Recei ved for revi ew Apri l 24, 1995. Revi sed manuscri pt
recei ved March 13, 1996. Accepted March 21, 1996.
X
Thi s
study was suppor ted by the Fr ench County Counci l of
Burgundy.
JF950239C
X
Abstract publ i shed i n AdvanceACS Abstracts, May
15, 1996.
1408 J. Agric. Food Chem., Vol. 44, No. 6, 1996 Douzals et al.