Can. lnsf. Food Sci. Techno/. J. Vol. 23, No. 2/3. pp.

'25130, 1990

RESEARCH

Degradation Kinetics of Thiamine in Aqueous Systems

at High Temperatures
H. Ramaswamy', S. Ghazala2 and F. van de Voort
Department of Food Science and Agricultural Chemistry
Macdonald College of McGill University, Box 187
Ste Anne de Bellevue, PQ, H9X ICO, Canada

levels of nutrients while achieving the desired degree

of microbiological sterility (Lund, 1975). This
requires accurate data on reaction rate kinetics at
appropriate temperatures. Thiamine is a relatively
heat labile vitamin that has been used as a chemical
index of sterility in some studies (Mulley et al.,
1975a,b,c; Guzman-Tello and Cheftel, 1987). There
have been several studies on the thermal destruction
kinetics of thiamine (Greenwood et al., 1944; Bendix
et al., 1951; Cameron, 1955; Feleciotti and Esselen,
1957; Everson et al., 1964; Lenz and Lund, 1977;
Dennison et al., 1977; Skjoldebrand et al., 1983;
Leonard et al., 1986; Fernandez et al., 1986). As
tabulated in two recent reviews (Thompson, 1982;
Villota and Hawkes, 1986), data on thiamine
degradation generally reveal first order reaction rate
kinetics with associated activation energies in the
range of 33 to 124 kJ/mole. Some results (Booth,
1943; Farrer and Morrison, 1949; Farrer, 1945, 1955;
Sabrie et al., 1968; Dwivedi and Arnold, 1973) also
indicate that the type of food product, temperature
range, oxygen level and several other factors
influence the degradation kinetics of thiamine.
Perhaps, thiamine is one of the most widely studied
vitamins from thermal degradation viewpoint, but
even so, only a few studies have been carried out on
its heat destruction in aqueous solutions (Mulley et
al., 1975a,c; Guzman-Tello and Cheftel, 1987).
The majority of studies on thiamine degradation
kinetics are based on real foods subjected to various
unit operations such as thermal processing, concentration, freezing and drying as well as storage at
different conditions of temperature, moisture content
and water activity. For the purpose of thermal
process optimization the majority of literature data
discussed earlier are of limited value unless applied
under the reported conditions because of the large
number of variables associated with them.
The objective of this research was to obtain kinetic
data for high temperature thermal destruction of
thiamine in water, as well as in a mixture containing
an additional vitamin (ascorbic acid) and color
forming compounds (glucose and glycine). The
purpose was to obtain data needed for the verification of thermal process simulations.

Abstract
High temperature thermal destruction kinetics of thiamine (BI)
were studied in water and in an aqueous mixture of thiamine,
ascorbic acid and Maillard color forming compounds glucose and
glycine. The thiamine content of test samples sealed in glass
ampoules and capillary tubes subjected to various time-temperature treatments was analyzed by HPLC. The study indicated that
the two sample heating techniques (ampoule and capillary) were
comparable; the destruction of thiamine could be described by
first order reaction rate kinetics, and the destruction behavior was
dependent on the presence of other compounds (ascorbic acid and
color precursors). The activation energy and reference rate
constant (k o) at 121.I o C for thiamine destruction using the
Arrhenius approach ranged from 103-118 kJ/mole and 0.00600.0067 minot in water, and 71.1-73.4 kJ/mole and 0.0066-0.0069
min t in the mixture, respectively. Similar analyses using the TDT
approach yielded z and Do values of 26.4-30.6 Co and 350-394
min in water and 42.4-43.8 Co and 338-354 min in the mixture,
respectively.

Resume
Les cinetiques de destruction thermique a haute temperature de
la thiamine (B,) furent etudiees dans I'eau et dans un melange
aqueux de thiamine, d'acide ascorbique et de precurseurs de la couleur Maillard, Ie glucose et la glycine. La teneur en thiamine fut determinee par HPLC sur des echantillons scelles dans des ampoules de
verre ou dans des tubes capillaires, soumis a divers traitements de
temps-temperature. D'apres les resultats, les deux techniques de
chauffage (ampoule et capillaire) furent com parables. La destruction de la thiamine pourrait etre decrite par des cinetiques de vitesse
de reactions de premier ordre, et Ie comportement de la destruction
fut en fonction de la presence de d'autres constituants (acide ascorbique et precurseurs de couleur). L'energie d'activation et la constante de vitesse de reference (k o a 121.1 C pour la destruction de
la thiamine utilisant I'approche Arrhenius oscillerent entre 103-118
kJ/mole et 0,0060-0.0067 min-I dans I'eau, et 71.1-73.4 kj/mole
et 00.0066-0.0069 min - I dans Ie melange, respectivement. Des
analyses similaires utilisant I'approche TDT donnerent des valeurs
z et Do de 26.4-30.6 C et 350-394 min dans I'eau, et 42.4-43.8 C
et 338-354 min dans Ie melange, respectivement.

Introduction
Thermal processing is an important method of
extending the shelf-life of foods in hermetically sealed
containers. Although both micro-organisms and
quality factors are degraded by heat, their relative
sensitivity to thermal destruction at various temperatures makes it possible to retain selectively higher
ITo whom correspondence should be addressed
2Department of Agricultural Engineering

125

Experimental
Sample preparation
Test solutions containing thiamine (thiamine
hydrochloride, Canlab Canada, Montreal, PQ) were
prepared in double-distilled water (DOW) as follows:
a) thiamine in water (Bl/DDW: 0.1 g thiamine
dissolved in one litre of DOW, and b) thiamine in a
mixture (Bl/MIX): 0.1 g thiamine, 1.0 g L-ascorbic
acid, 10.0 gO-glucose and 8.0 g glycine dissolved in
one litre DOW.

Kinetic set-up
The kinetics of thermal destruction of thiamine in
aqueous solutions were studied at selected temperatures both individually (Bl/DDW) and in mixtures
(Bl/MIX). Two different techniques were employed
to subject test samples to different time-temperature
treatments: 1) Ampoule technique and 2) Capillary
tube technique.
In the ampoule technique, the experiments were
carried out with 4-mL aliquotes of aqueous test
samples (at natural pH) in lO-mL glass ampoules
(Canlab Canada, Montreal, PQ) with the tips sealed
using an oxygen-natural gas flame. For each test run,
24 sample-sealed ampoules were placed in a wire
basket in individual compartments and the basket
was placed into a circulating oil bath maintained at
the desired temperature. The samples were heated for
various predetermined time intervals while the hot
oil circulated vigorously in the bath (temperature
stability 0.2C). Two ampoules were quickly
removed from the bath at the end of each time
interval and immediately plunged into an ice water
bath for quick cooling. The samples from all test
ampoules (plus two unheated samples) were individually analyzed for their thiamine content (details
follow).
In the capillary tube technique, 100 JLL samples of
test solutions were inserted into thin walled, glass
capillary tubes (90mm length, 1.8 mm 00, 0.15 mm
wall thickness; Canlab Canada, Montreal, PQ) using
a micro-syringe. The tubes were then sealed in a gas
flame. For each test run, 48 capillary tubes were
employed. The basket containing the capillary tubes
was introduced into the circulating oil bath and
heated as outlined previously to various predetermined times. Four tubes were quickly removed from
the bath at the end of each time interval and
immediately plunged into an ice water bath for quick
cooling. Two such tubes were required for each
thiamine analysis and two analyses were performed
for each time-temperature combination.

Estimation of thiamine
Thiamine content was estimated by a high pressure
liquid chromatography technique using a Waters
HPLC system (Waters Chromatography Division,
Millipore Corp., Milford, MA) consisting of WISP
Model 71 OB Intelligent Sample Processor, Model 510
126 / Ramaswamy et al.

HPLC Pump, Model 441 Absorbence Detector and

a QA-l Data Analysis System. The chromatography
column was a wBondapak Cl8 3.9 mm x 30 cm
stainless steel column with a Guard-Pak Precolumn
(end capped) with a mobile phase of methanol:water
(25:75) containing 200/0 low UV PIC B6 (hexane
sulfonic acid) at a flow rate of 1 mL/min. The
detector was set to 254 nm with 0.1 absorbance unit
full scale and the sample injection was 15 JLL. The
retention time for thiamine was 9.0 min. The data
processor was programmed to print the area for the
test peak (9.0 min) directly in thiamine concentration
based on previously stored calibration values using a
standard test solution.

Data gathering and analyses

The kinetic studies were carried out at temperatures of 110, 120, 130, 140 and 150C, to cover the
temperature range of interest in both conventional
and high temperature (UHT) thermal processing
operations.
Residual thiamine content in samples following
heating for various time intervals at a given
temperature were expressed as percentage of the
initial thiamine content by dividing the concentration
of thiamine at any time by the concentration of
thiamine at time zero (no heating). The retention (%)
data at a given temperature was analyzed based on
a first order reaction rate. To evaluate reaction rate
parameters, a linear regression was performed on the
natural logarithm of retention vs time to obtain the
slope. The reaction rate constant, k, and the decimal
reduction time, 0, were obtained using the following
relationships based on first-order reaction rates:
k = -regression slope

(I)

D = -2.303/k

(2)

The temperature sensitivity of the reaction rate

constants were analyzed by both Arrhenius and TOT
techniques. In the Arrhenius technique, the activation energy (EJ was obtained from the regression
slope of In (k) vs reciprocal of absolute temperature
(OK!):
Ea

-(slope) x R

(3)

where: R is the gas constant.

In the TOT method, the z value was obtained from

the regression slope of 10g(O) vs temperature (0C)
and:
z

-l/(slope)

(4)

The R2 values from the above regression equations

were used to compare the usefulness of the two
techniques for describing the destruction behaviour
of thiamine.
J. [nst. Can. Sci. Technol. Aliment. Vol. 23. No. 2/3. 1990

5.0,.,.-------------------,

5.0,::---------------------,

4.0

4.0

ai'
c 3.0

110D C

120 DC

130DC
0
0

140 DC

1.0

1.0

150 C

0.0 '----100

50

150

200

---'50

---'100

.1.-

150

-'

200

Heating Time (min)

Heating Time (min)

Fig. 1. Retention of thiamine in water following various timetemperature treatments using the ampoule heating technique.

Fig. 2. Retention of thiamine in water following various timetemperature treatments using the capillary heating technique.

Results and Discussion

Activation energy and z values:

thiamine in water

Kinetics of thiamine destruction in water

The destruction pattern of thiamine in aqueous
solutions over the temperature range of 110 to I50 D C
essentially indicated a first-order (semi-logarithmic)
reaction rate for the thermal destruction of thiamine
both by the ampoule and the capillary techniques
(Figures 1 and 2). The regression analysis (Table 1)
also indicated that the R2 values (greater than or
equal to 0.97) associated with the kinetic data at
various temperatures were very similar with the
ampoule and capillary techniques. The reaction rate
constants, k and D values, obtained from the
regression slopes (equations 1 & 2) at various
temperatures as obtained by the two techniques
(ampoule and capillary) were generally comparable
(Table 1). The ampoule technique was originally
employed based on its similarity to the various TDT
techniques (Stumbo, 1973). The capillary technique
was included primarily as an alternative for use at
higher temperatures (130-I50C) which could potentially involve short heating times. Practically instantaneous heating times were possible with the capillary
technique due to the extremely small diameter of
these tubes and the small sample size. For situations
involving high temperature short time heating, the
capillary technique would offer a better choice over
the ampoule technique. In the present studies,
however, since the heating times were found to be
relatively long even at higher temperatures, there was
no special advantage with the capillary technique
over the ampoule technique. But, the study
demonstrated that the capillary technique for nutrient
degradation studies was feasible and could be
conveniently employed should there be any need.
Can. lnsl. Food Sci. Technof. J. Vol. 23. No. 2/3. 1990

The temperature sensitivity of the reaction rate

constant, k, was evaluated by the Arrhenius concept
with data from both ampoule and capillary techniques (Figure 3). The regression analysis (Table 2)
again indicated comparable results with both capillary and ampoule heating techniques (R 2 = 0.96 in
the ampoule technique as compared with 0.94 in the
capillary technique). The associated activation energies were 118 kllmole (ampoule) and 103 kllmole

Table 1. Kinetic parameters for thiamine degradation

Sample
Method
description

Temperature

R2

(0C)

k value D value
(min-I
(min)

Ampoule

110
120
130
140
150

0.9927
0.9803
0.9654
0.9944
0.9955

0.0015
0.0069
0.0181
0.0302
0.0568

1509
333.1
127.0
76.3
40.5

Capillary

110
120
130
140
150

0.9804
0.9807
0.9799
0.9978
0.9840

0.0020
0.0073
0.0187
0.0324
0.0406

1167
313.5
123.2
71.0
56.8

Thiamine Ampoule
in mixture

110
120
130
140
150

0.9958
0.9951
0.9942
0.9960
0.9910

0.0032
0.0065
0.0116
0.0190
0.0260

717.1
354.0
197.8
121.2
88.5

Capillary

110
120
130
140
150

0.9922
0.9930
0.9936
0.9990
0.9954

0.0034
0.0069
0.0121
0.0194
0.0302

682.7
334.4
190.0
119.0
75.8

Thiamine
in water

Ramaswamy et al. / 127

-2.0,---------------------,

3.5 , - - - - - - - - - - - - - - - - - - - ,

81IDOW(Amp)

81/DOW(Amp)

--

--

81IDOW(Cap)

-3.0
o

81/DOW(Cap)

81/MlX(Amp)

3.0

811....X(Amp)

y::-

81/tdX(Cap)

.~

BlIM1X(Cap)
8

E -4.0

"""""""'t--..

Q)

::l

iil 2.5
>

~ -5.0
jO

2.0

-6.0
o

-7.0

L-

0.0023

L.-

0.0024

L.-

.L......_ _-----J

0.0025

1 .5 '------'----'-----'----'---"------'
100
110
120
130
140
150
160

0.0027

0.0026
1

Reciprocal Temperature (0 1\ )

Temperature (oC)

Fig. 3. Arrhenius-plot of thiamine destruction in water and in an

aqueous mixture employing both ampoule and capillary
heating techniques.

Fig. 4. TOT-plot of thiamine destruction in water and in an

aqueous mixture employing both ampoule and capillary
heating techniques.

(capillary). Reference k values at 121.1 C (k o) found

from the regression equations were: 6.0 x 10-3 min- I
(ampoule) and 6.7 x 10-3 min-I (capillary). Similar
regression analysis of D values vs temperature using
the TDT concept (Figure 4) also yielded comparable
results with the two techniques (Table 2) with
associated z values of 26.4 Co (ampoule) and 30.6 Co
(capillary). The reference D values (Do) were 394 min
(ampoule) and 350 min (capillary), respectively. The
two techniques (ampoule and capillary) differed in
the evaluated E a and z values by up to 7.2070 from
their midpoint value. A statistical analysis using the
t-test showed no significant difference (p > 0.05) for
the kinetic parameters obtained at a given temperature (k and D value evaluation) or their temperature
dependence (E a and z value evaluation) between the
ampoule and capillary techniques.
The regression analyses of the temperature functions (E a and z values) of reaction rate constants gave
similar R2 values (Table 2) indicating that the
Arrhenius and TDT techniques were comparable in
describing the temperature dependence of the kinetic

parameters. This is in contrast to the fact that in one

technique (TDT), the kinetic parameter D is assumed
to be directly proportional to the temperature while
in the other (Arrhenius) the k value is assumed to be
dependent on the reciprocal of absolute temperature.
The relatively high R2 values found with reference to
the TDT and Arrhenius concepts may be misleading
to some extent. A closer observation of Figures 3 and
4 shows some nonlinearity of the temperature
dependence with the curves being a bit convex
upward with the Arrhenius and concave upward with
the TDT technique. This implies that both these
techniques are somewhat less than satisfactory in
describing the temperature dependence of the
parameters. The relatively large standard errors
(Table 2) also support this observation. It should be
noted that the high standard errors were due to the
linearization of the curve and not due to experimental
errors (variation between replicate value were mostly
less than 5%).
The results of the study compared favorably with
published literature values although the majority of

Table 2. Arrhenius and thermal death time (TOT) parameters for thiamine destruction in aqueous solutions in the temperature range
of 110-150C.
Sample
description
Thiamine
in water
Thiamine
in mixture

Method

E,

Ampoule

(kJlmole)
118.0

Capillary
Ampoule

R2a

t~.95

R2b

ko
(min- I

3.4

0.92

5.1

349.5

0.0067

0.98

3.6

354.3

0.0066

2.4

337.8

0.0069

(CO)

0.96

26.4

0.95

102.6

0.94

15.2

30.6

71.1

0.99

4.6

43.8

(CO)

Capillary
73.4
0.99
3.0
42.4
0.99
'R 2 Variance with the Arrhenius method; bR 2 Variance with TOT method; CtO.95 = standard error.

128 / Ramaswamy et al.

t~.95

00
(min)
394.3

(kJ/mole)
13.7

0.0060

J. InSf. Can. Sci. Technol. Aliment. Vol. 23. No. 2/3. 1990

5.0 r - - - - - - - - - - - - - - - - - ,

5.0 r - - - - - - - - - - - - - - - - - - - - ,

4.0

4.0

~
3.0
B
c:

,gc:

Q)

Q)

a:
X
~ 2.0
......
,...

a:
X

~
......
r

2.0

l;Q.

l;Q.

'"

3.0

Q)

Q)

'"
1.0

1.0

0.0 '--_.....L_ _'--_-'--_ _............_-'--_ _'--_--'

100
150
200
250
300
350
o
50

Heating Time (min)

0.0 '--_--'-_ _'--_--'-_----.C............_-'--_----l'--_---J

50

100

150

200

250

300

350

Heating Time (min)

Fig. 5. Retention of thiamine in an aqueous mixture following

various time-temperature treatments using the ampoule
heating technique.

Fig. 6. Retention of thiamine in an aqueous mixture following

various time-temperature treatments using the capillary
heating technique.

published data involved real foods where the

destruction behavior depended on several factors in
addition to heat. Feleciotti and Esselen (1957)
reported E a values for thermal destruction of
thiamine in the range of 115-l20 kJ/mole in pureed
carrot, green beans, peas, spinach, beef heart, beef
liver, lamb and pork. Bendix et al., (1951) reported
E a values of 86-92 kJ/mole for whole peas
(brine/vacuum-packed) during heat processing at
104-132C. For pea puree, Lenz and Lund (1977)
found an E a of 97 kJ/mole (115-138C) while Mulley
et al. (1975a) reported somewhat higher values of
113-116 kJ/mole for both pea and beef purees
(121-138C). For pork puree, Greenwood et al.
(1944) reported much lower E a value of 77 kJ/mole
while Skjoldebrand et al. (1983) found an E a value
of 114 kJ/mole for the same. Fernandez et al. (1986)
also found that the Ea values associated thiamine loss
were in the range of 98 - 116 kJ/mole in model
systems containing various solutes with the water
activity was adjusted to 0.95. In the lower temperature region (storage studies), the associated E a values
for thiamine destruction have been reported in the
range of 33-101 kJ/mole (Cameron, 1955). In
phosphate buffer at pH 6.8, Guzman-Tello and
Chefte! (1987) reported an E a value of 94 kJ/mole
for thiamine destruction. On the other hand at a pH
6.0 in phosphate buffer, Mulley et al. (1975a) found
an E a of 124 kJ/mole. The E a values of 102-118
kJ/mole found in the present studies were within the
domain of published values.

Kinetics of thiamine destruction

in a mixture

Can. Insl. Food Sci. Technol. J. Vol. 23. No. 2/3. 1990

In order to further explore the influence of other

compounds on the degradation behavior of thiamine,
a simple food model was formulated using an
additional nutrient, ascorbic acid, and Maillard-color
forming compounds, glucose and glycine. The
thiamine destruction in this system (B 1/MIX) was
evaluated parallel to Bl/DDW which included only
thiamine.
The destruction pattern of thiamine in Bl/MIX
over the temperature range of 110 to 150C also
demonstrated first-order reaction rates as determined
by the ampoule and the capillary techniques (Figures
5 and 6). The regression analysis (Table 1) again
indicated similar R2 values; the magnitudes of the
reaction rate constants, however, differed from their
counterparts in Bl/DDW.

Activation energy and z values in mixture

The temperature sensitivity of the reaction rate
constants (k) and D values (Figures 3 & 4) gave E a
values in the range of 71.1 to 73.4 kJ/mole and z
values in the range 42.4 to 43.8 CO (Table 2).
Reference k values ranged from 6.60 x 10. 3 to 6.90 x
10-3 min- l while the reference D values varied from
338 to 354 min. With both E a and z values, the two
techniques (capillary and ampoule) differed only by
a 1.5010 margin from their midpoint value. In
Ramaswamy et at. / 129

contrast to the destruction behaviour of thiamine in

water, thiamine destruction in the mixture showed a
better linear fit of data with reference to both
Arrhenius and TDT techniques and obviously the
associated standard errors were much smaller (Table
2).

A striking difference between the destruction

behavior of thiamine in Bl/DDW and Bl/MIX was
the lower Ea and higher z value associated with the
Bl/MIX which indicates a relatively better temperature stability. Temperature increases of 42-44Co were
needed to result in a ten-fold increase in the rate of
destruction of thiamine in the mixture as compared
with 26-30Co in the pure system. However, the
decimal reduction times at the reference temperature
(l21.ICO) were somewhat comparable in the range
338-394 min. It is difficult to precisely explain these
differences, but several simultaneous reactions taking
place in the mixture would undoubtedly influence the
destruction pattern of individual components. There
could also be interactions between the components,
for example, ascorbic acid which is often used as an
antioxidant and presence of sugar may offer some
protection against the destruction of thiamine at
elevated temperatures. Comparison of the results
with published literature was not possible because
similar data were unavailable.

Conclusions
The two sample heating techniques (ampoule and
capillary) employed in the kinetic studies gave
comparable results. The study confirmed that the
thermal destruction of thiamine in aqueous solutions
could be adequately described by first order reaction
rate kinetics. The TDT and Arrhenius concepts were
similar in describing the temperature dependence of
the kinetic parameters.
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Submitted August II, 1989
Revised October 13, 1989
Accepted December 16, 1989

J. [nsf. Can. Sci. Technol. Aliment. Vol. 23. No. 2/3, 1990