Analysis and Stability of the Sweetener Sucralose

in Beverages
M. E. QUINLAN and M. R. JENNER

ABSTRACT formualtions,.at pH 2.7 and pH 3.0, were evaluated for sucralose

stability. The pH values were chosen to correspond to those of a
The stability of the sweetener sucralose in a Lange of prototype bev- regular cola product and of a low calorie product. The lower pH was
erages was confirmed. Storage conditions were chosen to encompass achieved by the addition of phosphoric acid.
the typical shelf life of the products under investigation plus some
extreme conditions. The methods developed for the analysis of the
beverages used high performance liquid chromatography with refrac- Storage conditions
tive index detection. The reproducibility of each method was deter-
mined by means of recovery experiments. Stored samples were also Samples were stored as indicated in Table 1. The storage conditions
subjected to sensory evaluation. Sucralose was stable under all the were designed to encompassthe typical shelf life of the products under
conditions tested thus demonstrating the potential suitability of this investigation plus some extreme conditions. The cola samples stored
sweetener in soft drinks. in the dark were placed in constant temperature rooms and the ex-
posure to sunlight was achieved by standing the samples in a. west
facing window. The coffee was maintained at 80°C in a vacuum flask.
INTRODUCTION Blank (unsweetened)products were also stored under identical con-
ditions for use in the analysis and sensory evaluation was performed
WHEN FOOD PRODUCTS and beveragesare sweetenedwith at each sampling point.
high intensity sweeteners, it is important to determine that the
products have adequateshelf lives and that there is no effective
loss of sweetness under the anticipated conditions of use or Sampling intervals
storage. Sucralose is a high intensity sweetener derived from Samples were removed at regular intervals throughout the storage
sucrose (chemical formula C,,H,,O,Cl,) and is approximately period and submitted for HPLC and sensory analysis. The sampling
600 times sweeter than sugar. One of the major potential uses times for each of the products are indicated in Table 2.
of sucralose is in soft drinks. Studies were therefore undertaken
to confirm the stability of this product in a range of prototype
beverages. Analysis
The determination of high intensity sweeteners such as as- The analytical method for each beverage under investigation was
partame and saccharin in soft drinks is now well documented evaluated by spiking a blank (i.e., unsweetened)formulation with the
(Beckman and Webb, 1984; Williams, 1986), and most meth- appropriate level of sucralose. The spiked samples (6-10) were then
ods employ reverse phase HPLC with UV detection. Sucra- taken through the analytical procedure and the recovery factors de-
lose, however, being a derivative of sugar is unsuited to detection termined. The variation in results obtained for the recovery factors
by UV except at low wavelengths and so a different method gave a measure of the reproducibility of the method.
Sample preparation. Cola sampks (l;om early sampling p&Us).
of detection was required. Methods were therefore developed Approximately 20 mL of cola sample were poured into a clean glass
using HPLC with refractive index detection. beaker. The beaker was then placed in an ultrasonic bath for 10 min
The objective of this study was to demonstrate the stability to ensure complete decarbonation of the sample. A CIR Sep Pak car-
of sucralose in prototype beverages and to this end samples tridge (Waters Assoc.) was activated by the injection of 2 mL meth-
were stored under conditions designed to encompassthe typical anol followed by 5 mL water. A 10.0 mL aliquot of the dccarbonated
shelf life of the product plus some extreme conditions. In ad- cola sample was then slowly injected onto the Sep Pak, discarding
dition to the HPLC analysis, the stored samples were subjected the eluent. The cartridge was washed with 5 mL of water, discarding
to sensory evaluation to confirm that no loss of sweetness had the eluent. One milliliter of air was then injected to ensure that all the
occurred during storage. water had passed through the cartridge before eluting the sucralose
with 5 mL of methanol and collecting the cluent. Again, 1 mL of air
was injected. The methanol extract was taken to dryness under a
MATERIALS & METHODS
Sucralose Table 7 -Storaae conditions
Sucralose, batches KL/S/12 and 153014 (Tate & Lyle Speciality Product Storage conditions Storage time
Sweeteners, UK) were used for these studies. Purity was greater than Cola 35°C in the dark 9 months
99%. 20°C in the dark 12 months
20°C in the light 4 weeks
Cola (second study) 20°C in the dark 26 weeks
Beverages Lemon/lime 20°C in the light 4 weeks
Coffee 80°C 24 hours
The prototype carbonated beverageswere formulated and produced
by the Product Development Department of Tate & Lyle. Both sweet-
ened (with sucralose) and unsweetened products were prepared. The Table l-Sampling intervals
beveragesunder investigation were, carbonatedcola containing 0.026%
Product Sampling intervals
sucralose (pH 2.8), carbonated lemon/lime containing 0.024% sucra-
lose (pH 3.8), and instant black coffee containing 0.007% sucralose. Cola 35°C (dark) 0, 1, 3, 6, 9 months
A second cola study was set up at a later stage in which two cola Cola 20°C (dark) 0, 1, 3, 6, 9, 12 months
Cola 20°C - second study 0, 5, 10, 18, 26 weeks
Cola 20°C (light) 0, 1, 2, 4 weeks
Authors Quinlan and Jenner are with Tate & Lyle Specialty Lemon/lime 20°C (light) 0, 1, 2, 4 weeks
Sweeteners, P.O. Box 68, Reading, Berks, RG2 2BX, UK. Coffee 80°C 0, 24 hours

244-JOURNAL OF FOOD SCIENCE-Volume 55, No. 1, 1990

stream of air at room temperature. The residue was then re-dissolved
in 2.0 mL distilled water and filtered through a 0.45~~filter prior to
analysis by HPLC.
HPLC analysis. All the prepared samples were analyzed using a
Waters HPLC system equipped with a refractive index detector (model
401 or model 410). The analytical column was a Cra reversed phase
Rad Pak cartridge (Waters Associates) and the mobile phase, a water/
methanol mixture (70%/30%). A flow rate of about 1 mL/min was
used to give a retention time for sucralose of approximately 8 min.
Injections of 1OOkL were made. A typical chromatogram is shown in
Fig. 1.
Lemonllime samples and cola samples (from later sampling points).
Approximately 20 mL of sample were poured into a clean glass beaker
which was then placed in an ultrasonic bath for about 10 min. to
ensure complete decarbonation of the sample. The sample was filtered
through a 0.4511filter and the filtrate analyzed by HPLC.
Cojj%e samples. Approximately 6 mL of coffee were passedthrough
an Alumina A Sep Pak cartridge (Waters Associates) and then through
a 0.45~ filter. The filtrate was analysed by HPLC.
Sensory analysis
Sensory assessmentof the samples was carried out by a standard
triangle test (International Standards, 1983), using a trained, experi-
enced panel selected from the local community. At zero time (control)
and at each sampling point sucralose was added to the sample “stored
without sucralose” at the level of the zero time samples (as determined
by the analytical results). The “sucralose added after storage” product
Carbonated Cola - 12 months 20°C
sucralose
Retention Time (min)
Fig. 1- Typical chromatograms of cola samples. Conditions are described in the text. The additional
11.9 min was due to another component in the cola sample, possibly benzoic acid.
Volume
was then compared to the “stored with sucralose” product to identify
any sensory differences between the products.
Panelists (between 34 and 41 people) were given three samples,
two identical and one different. Half the panelists were given two
“stored with sucralose” samples, the other half received two “stored
without sucralose” samples. The order of presentation was balanced.
Panelists were asked to try and identify the odd sample and to describe
the difference.
By directly comparing the “stored with sucralose” product and the
“stored without sucralose” product (with sucralose added at the zero
time level), any sensory differences such as sweetness loss, flavor,
appearanceor texture changes, caused by breakdown of sucralose or
interactions with other ingredients, could be identified.
RESULTS
HPLC analysis
Refractive index detection, which is extensively employed
for the analysis of sugars, was found to be suitable for the
analysis of sucralose in the beverages under investigation. Al-
though UV detection at 190 nm is satisfactory for sucralose in
aqueous solution, too much background interference was en-
countered with most food product extracts. It was necessary,
however, during the initial stage of the work to include a con-
centration step in the procedure for the carbonated cola samples
to attain a sufficient peak size for reliable measurement. This
was achieved by means of a C,, solid phase extraction car-
Carbonated Cola - Blank
Retention Time (min)
peak observed at approximately
I
55, No. 1, 1990~JOURNAL OF FOOD SCIENCE-245
I ANALYSIS AND STABILIN OF SUCRALOSE IN BEVERAGES. ..
Table J-Recovery factors determined to evaluate the reproducibility of Table 5-Stability of sucralose in beverages exposed to sunlight
the analytical methods
% Sucralose
Product Recovery factor
Storage time Cola Lemon/lime
Cola 84.5% c 2.5% (method 1)
100.7% + 1.5% (method 2) Zero time 0.026 0.024
1 week 0.025 0.024
Lemon/lime 102.6% + 1.6% 2 weeks 0.029 0.024
Coffee 97.6% k 2.2% 4 weeks 0.027 0.023

Table 4-Stability of sucralose in cola samples stored at two Table B-Stability of sucralose in cola samples stored at 20°C
temperatures ppm Sucralose
% Sucralose Storage time pH 2.7 pH 3.0
Storage time 35°C 20°C Zero time 184 191
Zero time 0.026 0.026 5 weeks 182 198
1 month 0.029 0.028 10 weeks 183 192
3 months 0.030 0.031 18 weeks 183 194
6 months 0.026 0.026 26 weeks 184 194
9 months 0.025 0.026
12 months 0.026

In no case was a significant difference detected between the

tridge which allowed a five fold increase in concentration. The
introduction of a new RI’detector (model 410) with a greater
sensitivity part way through the study, however, allowed the
elimination of the concentration step from the cola method. In
the case of the coffee, samples were passed through an Alu-
mina A cartridge to effect sample clean up prior to the HPLC
analysis.
The recovery factors determined to evaluate the analytical
methods for the beverages under investigation are summarized
in Table 3. It can be seen that the elimination of the concen-
tration step from the cola method resulted in an improved re-
covety factor of 100% and a lower coefficient of variation.
The results from the carbonated drink storage trials are given
in Tables 4 to 6. The sucralose concentrations represent mean
values from replicate analyses. The slightly high results ob-
tained for the cola samples at the 1 month and 3 month sam-
pling points were thought to be due to the poor reproducibility
of the original method. The second cola study gave much more
consistent results (Table 6).
No loss of sucralose was detected in the coffee study with
both the zero time and the 24 hr samples being found to contain
0.007% sucralose.
Sensory analysis
For each triangle test panel carried out, the number of panel-
ists correctly identifying the odd sample were totalled. Follow-
ing standard procedures (International Standards, 1983), one
third of the panelists who said they were unable to pick out an
odd sample were added to this total. Standard triangle taste
tables were used to determine the 5% or 1% level of signifi-
cance.
“stored with sucralose” and “stored without sucralose” prod-
ucts. This demonstrated that there had been no loss of sweet-
ness nor any interaction with other ingredients in the products
during storage.
CONCLUSION
THE HPLC RESULTS showed that there were no significant
changes in the sucralose level of any of the products investi-
gated. These results were corroborated by the sensory data
demonstrating that there had been no loss of sweetnessnor any
interaction with other sample ingredients during storage.
The data indicated that coffee and carbonatedcola and lemon/
lime beverages, sweetened with sucralose would maintain the
same intensity and quality of sweetnessthroughout normal shelf
life periods. This is particularly pertinent in the case of car-
bonated soft drinks which are traditionally formulated at low
PI-I.
The fact that no loss of sucralose was detected when the
products were subjected to elevated temperatures established
the stability of this sweetener and indicated its potential for
use in certain beverages.
REFERENCES
Beckman, D.D. and Webb, N.G. 1984. Reverse phase liquid chromato-
graphic determination of aspartame in beverages in beverage mixes. J.
Assoc. Anal. Chem. 67: 510.
International Standards. 1983. Sensory analysis methodolo p tfianylar
test. IS0 4120. International Organization for Standar izatron, Case
postale 56, CH-1211, Geneva, Switzerland.
Williams, W.L. 1986. Rapid separation of soft drinks ingredients using
HPLC. Food Chem. 22: 235.
MS received 6124188; revised 5/2/89; accepted 5/4/89.

246~JOURNAL OF FOOD SCIENCE-Volume 55, No. 1, 1990