337
Journal of Food Protection, Vol. 52, No. 5, Pages 337-342 (May 1989)
Copyright© International Association of Milk, Food and Environmental Sanitarians
Migration of Poly(ethylene terephthalate) (PET) Oligomers from
PET Plastics into Foods during Microwave and Conventional
Cooking and into Bottled Beverages
LAURENCE CASTLE, ALAN MAYO, COLIN CREWS and JOHN GILBERT*
Ministry of Agriculture, Fisheries and Food, Food Science
Laboratory, Haldin House, Queen Street, Norwich NR2 4SX (U.K.)
(Received for publication November 9, 1988)
ABSTRACT
The migration of total levels of poly(ethylene terephthalate)
(PET) oligomers into a diverse range of foods has been determined
using an analytical approach that involves hydrolysis of oligomers
to terephthalic acid, methylation, and analysis as dimethyl tereph-
thalate by stable isotope dilution GC/MS. Aspects of use of PET
materials examined in this study include roasting bags, PET trays
(for conventional and microwave oven use), and "susceptor pads"
for microwave browning applications. Total levels of migration of
PET oligomers were found to range from 0.02 to 2.73 mg/kg
depending on the foodstuff and the temperature attained during
cooking. On repeated-use of PET trays for heating olive oil there was
a decline in migration of oligomers from the first to second and
subsequent uses of the container. Migration of oligomers was found
to occur at only very low levels from PET bottles into alcoholic and
carbonated beverages.
Polyethylene terephthalate (PET) is a copolymer of eth-
ylene glycol with either terephthalic acid or dimethyl tereph-
thalate. It is used in the form of trays and dishes for microwave
and conventional cooking where the polymer will not ther-
mally deform below about 220°C, and in the form of a film for
oven roasting bags. PET also forms the food contact surface
layer in a new form of microwave packaging where the
polyester is metallized with vacuum deposited aluminium
which in turn is bonded to a board substrate. These materials
are termed "active" packaging or "susceptors," and are
intended for microwave use where high temperatures are
required locally for browning applications such as pastries,
potato fries, and popcorn. The most widespread application of
PET has, however, been in the form of stretchblown bottles for
carbonated beverages where the copolymer provides an effec-
tive barrier against carbon dioxide loss. PET miniature bottles
(50 ml) have also found use for packaging spirits for airlines
where a particular attraction has been the low weight of the
PET material compared to glass.
In addition to the physical properties that have made PET
desirable as a food contact material, it is also relatively free of
additives and adventitious low molecular weight constituents
and so has intrinsic low migration characteristics. When PET
JOURNAL OF FOOD PROTECTION. VOL. 52. MAY 1989
has been tested with global migration procedures using olive
oil as a food simulant, values have generally been low; ranging
from 0.7 mg/dm 2 after 10 d at 40°C to 4.0 mg/dm 2 after 2 h at
175°C (I). The presence of minor constituents in PET plastics
which may give rise to migration have however been scruti-
nized in some depth. Acetaldehyde can be formed by thermal
degradation of PET during polycondensation and melt proc-
essing, and levels are closely monitored in the plastic (6,15) as
trace amounts migrating can adversely affect the taste of cola
and other beverages. Migration of ethylene glycol from PET
bottles into 3% acetic acid food simulant stored for 6 months
showed levels of about 0.1 mg/kg (8), which are insignificant
in relation to the likely maximum level of 30 mg/kg of this
compound permitted in foods in the European Community by
migration from plastic materials and articles (7). Residual
monomer levels of 1.5 and 1.7 mg/kg terephthalic acid have
been found in PET film and bottles respectively (14), but
migration into food simulants was found to be <0.01 mg/kg for
water, acetic acid and 15% ethanol, and 0.02 and 0.03 mg/kg
for migration into 50% ethanol and into olive oil (14).
PET is also known to contain small amounts of low
molecular weight oligomers which mainly consist of cyclic
compounds ranging from dimer to pentamer (11). The levels
of these oligomers extractable from the polymer with meth-
ylene dichloride range from 0.06 to 1.0% w/w depending on
the type of PET (9). For solid-phase polymerized PET resin
containing the lowest amounts of extractable oligomers, 81 %
of the extract comprised cyclic trimer with the other compo-
nents being lower molecular weight linear oligomers. Meth-
ods of analysis of oligomers both in the PET resin and in
materials such as refrigeration oils have been reported (11,12)
and employ adsorption and gel permeation chromatography
as the basis of separating and monitoring the individual
components. Although the major constituents which are likely
to migrate from PET into foods are the oligomers, there are no
published reports of attempts to measure the migration of
these species. Due to the difficulties of developing analytical
procedures for measuring individual oligomers we report here
a method which involves conversion of all the oligomers
present in a food extract to the monomer terephthalic acid.
338 CASTLE, MAYO, CREWS AND GILBERT
This method has the disadvantage that oligomers are meas-
ured as total levels together with any monomer that may be
present, although published data suggests the monomer con-
tribution will be low (14). We have previously used with some
success this approach of degrading polydisperse migration
species to common low molecular weight units for the deter-
mination of polymeric plasticizers (3) and epoxidized soya
bean oil in foods (2). Prior experience with the use of stable
isotope-labelled internal standards both for determining the
above analytes, as well as for monomeric plasticizers (4,5,13)
and employing GC/MS for the determinative stage has dem-
onstrated the advantages of specificity and precision that can
be achieved. In the method reported in this paper we have
chosen accordingly to employ deuterated terephthalic acid as
internal standard, and with GC/MS this has enabled a precise
and specific analysis of PET oligomers in a diverse range of
foods.
MATERIALS AND METHODS
Chemicals
Potassium hydroxide (Analar grade) and sulphuric acid (Aris-
tar grade) were obtained from BDH Chemicals Ltd. (Poole, Dorset,
U.K.). Boron trifluorideetherate (re-distilled grade) was from Sigma
Chemical Co. (Poole, Dorset, U.K.), isophthalic acid (98% pure),
terephthalic acid (98% pure), and deuterated (d4-) terephthalic acid
(98% deuterium incorporation) were from Aldrich Chemical Co.
(Gillingham, U.K.). All solvents (HPLC grade) were from Rathburn
Chemicals Ltd. (Walkerburn, Scotland, U.K.).
Calibration standards
A calibration standard comprising a mixture of PET oligomers
was prepared by chloroform reflux of 'Melinex' (Type 851 I) film.
After removal of the chloroform on the rotary evaporator the residual
solid was used for gravimetric preparation of calibration solutions.
For spiking into foods an oligomer mixture in olive oil was obtained
by extraction from PET trays at 175°C for 2 h. The concentration of
oligomers in the oil (ca. 60 mg/kg) was determined by the described
total digestion method using the chloroform extract for calibration.
The oil was employed for spiking experiments to establish the
oligomer recovery of the method for foods.
Samples
PET roasting bags and trays appropriate to household usage
were purchased from retail outlets. Susceptor materials were ob-
tained in the form of retail packaging containing pre-packed foods
as supplied for use in microwave cooking. PET bottles containing
carbonated beverages were retail samples, and spirit miniatures were
obtained as airline purchases. All foods intended for cooking in
contact with PET were purchased from local retail outlets, where it
was established that the products had not previously been in contact
with plastic materials. Olive oil was a rectified grade complying with
the specification for use as a food simulant for EC overall migration
testing.
Use of PET materials during microwave and conventional cooking
Foods that had not previously been in contact with plastic-
materials were placed in roasting bags or in trays and heated on the
middle shelf of a conventional domestic electric oven. The pre-
warmed oven was nominally set at 204"C (temperature measure-
ment revealed that the oven cycled between 190 and 210°C) and the
foods were heated according to the recipes or until sufficiently
JOURNAL OF FOOD PROTECTION, VOL. 52, MAY 1989
cooked by visual inspection. Microwave cooked foods were pre-
pared in a Sharp Carousel Model R-7400 oven with a nominal output
of 600W on high power.
Repeat-use experiments with PET trays
Pre-heated olive oil (30 g) was poured into PET trays giving a
depth of oil of about 1 cm and the sample was heated for 2 hat 175°C.
The oil was then removed by pipette for analysis, before performing
a repeat treatment on the tray. The experiment was repeated imme-
diately using the same tray a total of 5 times before a resting period
of 3 weeks followed by a further 3 migration exposures.
Analysis
The analytical method was based on the alkaline hydrolysis of
all PET oligomers to terephthalic acid. Deuterated terephthalic acid
was added as internal standard and, after methylation, the total
oligomer concentration was determined as dimethylterephthalate by
stable isotope dilution GC/MS. Beverage samples were initially con-
centrated by evaporation prior to hydrolysis, while for composite
food samples lipid extraction was carried out. In both instances the
deuterated internal standard was added immediately after the alka-
line hydrolysis. Composite food samples received an additional
clean-up stage after methylation to remove lipid components prior to
GC/MS analysis.
Sample preparation for composite foods
All glassware and materials in contact with solvents during the
assay were carefully washed with acetone prior to use. Food samples
after cooking were blended to a slurry in a domestic food processor
and sub-samples (30 g) were taken for analysis. Acetone/hexane (1:1
v/v,approx. 150 ml) and concentrated hydrochloric acid (1 ml) were
added to the food sample in a beaker and the mixture homogenized
with a Ultra-Turrax homogenizer for 2 min. The supernatant liquid
was decanted from the residue, which was then extracted twice with
further portions of solvent (150 ml). The extracts were combined and
dried over sodium sulphate. After gravimetric evaporation to dry-
ness, an accurately weighed portion (ca. 1 g) of the lipid extract was
transferred to a 24 ml crimp-top glass vial (F42 Perkin Elmer,
Beaconsfield, U.K.) and hydrolysed overnight by treatment with 0.2
M potassium hydroxide in methanol (4 ml). Extracts of foods
yielding less than 1 gof lipid, were transferred in their entirety to the
hydrolysis vial (containing from 1 to 20 |ig of d4-terephthalic acid)
using acetone, which was subsequently removed under nitrogen.
This was followed by 1 ml of boron trifluoride etherate, and the
mixture was heated for 3 h at 60"C. After quenching with 2M
aqueous sodium chloride solution (2 ml) the product was extracted
into diethyl ether, centrifuged and the upper phase transferred to a 4
ml screw-capped vial (Chromacol Ltd. London, U.K.). After blow-
ing down the extract to dryness under a stream of nitrogen, the
residue was taken up in dichloromethane/cyclohexane (1:1 v/v) to
give a solution containing about 0.3 g/ml of sample extract.
Size-exclusion chromatography (SEC) was carried out as de-
scribed elsewhere (10) using a 50 X 2.5 cm bed of Bio-Beads SX-3
(Bio-Rad, Watford, U.K.) operated at a flowrate of 0.5 ml/min of
dichloromethane/cyclohexane as eluent. Injections of 250 ul of
sample extracts were made and the fraction containing dimethyl
terephthalate (d - and d4-) was collected, evaporated to about 0.5 ml
and transferred to a small vial. Samples were stored at -20°C prior to
GC/MS analysis.
Sample preparation for beverages
All glassware and materials in contact with solvents during the
assay were carefully washed with acetone prior to use.
 MIGRATION OF PLASTICS INTO FOOD DURING COOKING
A sample of the beverage (10.0 g) was poured from the PET
bottle into a 24 ml crimp-top vial and reduced in volume to around
2 ml under a stream of nitrogen at 80-90"C. Potassium hydroxide
(0.6g) was then added and the sample capped and hydroly sed at 95°C
for 48 h with occasional shaking (Caution: gloves are required). The
following were then added to the vial: 6 M sulphuric acid (2 ml,
drop wise), d4-terephthalic acid 50 u.1 of 100 U-g/ml in aqueous
potassium hydroxide), and diethyl ether (12 ml). The vial was
capped, shaken to effect partitioning, and the lower aqueous phase
removed by pipette. The organic phase was dried over sodium
sulphate, decanted into a 24-ml vial, and evaporated almost to
dryness under a stream of nitrogen at room temperature (Caution: it
was important not to prolong nitrogen evaporation past dryness).
The residue was methylated by the addition of 2 ml of 10% boron
trifluoride (prepared from boron trifluoride etherate in methanol)
with reaction at 65°C for 3 h. The methylated solution was then
quenched by the addition of water (2 ml) and extracted with diethyl
ether (12 ml). The aqueous phase was removed from the vial by
pipette, the ether phase dried over sodium sulphate and evaporated
to around 0.5 ml under a nitrogen stream at room temperature. The
solution was stored at -20°C prior to GC/MS analysis.
Sample preparation for olive oil
A sub-sample of the oil (3.0 g) along with isophthalic acid
internal standard (10 u.1 of a 20 mg/ml solution in aqueous potassium
hydroxide) was hydrolysed with 0.2"M potassium hydroxide in
methanol (10 ml) at 65°C in a 24-ml crimp-capped vial. The reaction
period was for 3 h after homogeneity was attained (4-5 h in total).
Boron trifluoride etherate was added (2 ml) followed by a further
period of heating at 65°C for 5 h.
The methylation mixture was added to diethyl ether (40 ml) and
extracted with water (2 x 50 ml)-followed by aqueous sodium
sulphate solution (50 ml of a half-saturated solution). The organic
phase was dried over sodium sulphate and evaporated to dryness
under vacuum. The residue was dissolved in acetonitrile (50 ml) and
washed with hexane (3 X 50 ml). The acetonitrile phase was evapo-
rated to a small volume, made up to around 1 ml with chloroform, and
stored at -20°C until analysis by GC with an FID.
Selected ion monitoring GC/MS and GC (FID) analysis
GC/MS analysis was carried out on a Carlo Erba 4160 gas
chromatograph (MSE Instruments, Crawley, U.K.) directly coupled
to a VG 7070H mass spectrometer with a VG 11/250 data system
(VG Analytical Ltd. Manchester). Analysis was using a 30 m X 0.25
mm ID DB5 fused silica column (J & W Scientific Inc. Fulsom, CA
USA) operated isofhermally at 160"C with a helium carrier gas
flowrate of 1 ml/min using split injection (20:1). The mass spec-
trometer was operated in an electron ionization mode at a resolution
of 500 (10% valley definition). Ions at m/z 163 and 194 were
monitored for dimethyl terephthalate and the corresponding ions at
m/z 167 and 198 for the d,- internal standard. Dwell times were 80
msec per mass and a settling time of 20 msec to give a total cycle time
of 400 msec. Quantification was on the basis of peak areas. Calibra-
tion was carried out constructing a curve of the ratio of m/z 163/167
versus weight ratio of PET oligomers/internal standard.
GC analysis with an FID was carried out using a Carlo Erba
4160 gas chromatograph (MSE Instruments, Crawley, U.K.). The
column was a 25 m x 0.22 mm ID CP SIL 5CB (0.12 u.m film
thickness) fused silica column (Chrompack International B.V.)
operated at a hydrogen carrier gas flowrate of 2 ml/min. The tem-
perature was programmed from 120°C at 3"C/min to 130°C and then
held isothermally for 5 min; baking out the column at 250"C between
analyses. Injections (1 u.1) were made in the split mode with a 20:1
split ratio.
JOURNAL OF FOOD PROTECTION. VOL. 52, MAY 1989
339
RESULTS AND DISCUSSION
Performance of the analytical methods
Preliminary experiments with a chloroform extract from
PET showed that the theoretical yield of terephthalic acid,
based on the weight of oligomers taken, could be obtained on
hydrolysis. This demonstrated firstly, that no other species
had been extracted from the PET and secondly, the effective-
ness of the procedure in completely converting all the oligom-
ers to the parent acid. For calibration purposes this chloroform
oligomer extract was employed throughout, except for spik-
ing into foods where due to problems of solubility, an olive oil
extract containing PET oligomers was employed. The con-
centration of oligomers in this oil was directly determined
using the chloroform extract as a standard. All results are
expressed as mg/kg of total PET oligomers.
For the analysis of composite foods where a preliminary
extraction stage was employed, the deuterated internal stan-
dard was not added until after both the extraction and alkaline
hydrolysis. This step in the analysis was shown by spiking
various foods with oligomers at levels from 0.08 to 0.8 mg/kg
to have a mean recovery of 90%, and this figure was accord-
ingly used to correct subsequent data. After correction for this
initial recovery loss, the total assay for a variety of spiked
foods gave a found/added ratio of 98 + 8%. Reagent blanks for
the assay were <0.01 mg/kg and for each of the 12 food types
examined in the cooking experiments, blanks were in the
range <0.01 to 0.04 mg/kg with the exception of one sample
of lasagna which gave a blank value of 0.07 mg/kg. Blank
values were thus insignificant in relation to the measured
levels of oligomers in these composite foods.
For the analysis of beverages spiked at 0.1 mg/kg the
found/added ratio was 98 + 8%. Blank samples of water and
of beverages packed in glass showed levels <0.05 mg/kg.
Olive oil samples spiked at 10 mg/kg with oligomers and
analysed by the GC (flame ionization) approach gave found/
added values of 97 + 6%, with blank values below 0.5 mg/kg
(<0.02 mg/dm 2 ) the nominal limit of detection of the assay.
The mass spectrum of dimethyl terephthalate showed a
base peak at m/z 163 and a molecular ion at m/z 194 (25%),
with the deuterated internal standard showing analogous ions
at m/z 167 and 198. Although blank materials were generally
available, an additional confirmation of the specificity of the
assay was made by checking the ratio in each case of the two
respective ions. In no instance was there any evidence of
interference from co-extracted components from the foods in
their determination of the PET oligomers. Typical selected ion
chromatograms for a sample of French fries heated in contact
with PET in a susceptor and for a sample of vodka from an
airline spirit miniature PET bottle are shown in Fig. 1. Calibra-
tion curves were linear with a correlation coefficient of 0.9992
and did not differ in slope whether prepared directly from
standards or from spiking into food, thereby demonstrating
that no matrix effects were evident.
Migration of PET oligomers into foods
The results in Table 1 show migration levels of PET
oligomers in the range 0.02 to 2.73 mg/kg for a variety of foods
340 CASTLE, MAYO, CREWS AND GILBERT
TABLE 1. Migration of PET oligomers into foods during microwave and conventional cooking.
Food Type Cooking Article
Lasagne ~PET tray
Sausages PET tray
French fries PET tray
Baked beans PET tray
Stewed apple PET tray
Stewed cherries PET tray
Roast beef PET roasting bag
Roast pork PET roasting bag
Lasagne PET tray
Chicken curry PET tray
Peanut brittle PET tray
Pizza Susceptor pad
French fries Susceptor carton
Popcorn Susceptor carton
*Results for duplicate cooking experiments.
under different heating conditions. The levels observed were
influenced by the temperature and time of exposure, the extent
of contact with the food, and the nature of the food surface.
Results are reported for levels in duplicate migration experi-
ments. Where the food was homogeneous, such as for stewed
apple, the replication was good, but for composite heterogene-
ous foods such as lasagna, more significant differences were
observed reflecting the difficulties of preparing identical
replicate samples. Although the higher levels of migration
were observed for fatty foods, migration nevertheless still
occurred into aqueous foods such as stewed apple and baked
beans. Temperatures and times of exposure do appear for the
PET oligomers to be the dominant factors influencing migra-
tion, with the higher levels being observed after conventional
cooking at oven temperatures of 204°C for periods from 30 to
90 min, as opposed to somewhat lower migration levels
observed in microwave cooking in PET trays. For example,
for lasagna a ten-fold higher level of PET oligomer migration
was observed after conventional as opposed to microwave
cooking. In the latter case the cooking time was only 3 min and
the temperature in the food probably did not exceed 120°C
(unpublished data). For the examples of foods heated in pack-
aging including susceptor materials, although again the expo-
sure times were short, very high local temperatures were
generated as evidenced by charring of the paperboard sub-
strate. Although the layer of PET exposed to the food is very
thin in these susceptor applications, a level of oligomer
migration of 2.73 mg/kg was nevertheless observed in the case
of French fries microwaved in susceptor-carton, as opposed to
levels ten-fold lower for the same food heated in a conven-
tional oven in a PET tray. For popcorn in a susceptor-carton
the temperatures generated were again relatively high and
sustained for a longer period, but in this application the contact
time of the individual kernels of corn with the PET surface was
small, and the migration observed was accordingly low.
In Table 2 the results are presented for the migration of
PET oligomers into a variety of beverages including airline
spirit miniatures. For the aqueous beverages the oligomer
JOURNAL OF FOOD PROTECTION, VOL. 52, MAY 1989
Cooking Conditions PET Oligomers*
(mg/kg)
80 min at 204°C 0.78, 1.47
60 min at 204°C 0.40, 0.44
40 min at 204°C 0.35,0.27
30 min at 204°C 0.12,0.20
40 min at 204°C 0.19,0.21
40 min at 204°C 0.11,0.10
90 min at 204°C 0.82, 0.79
90 min at 204°C 0.38,0.80
Microwave 3 min high 0.18,0.07
Microwave 3 min high 0.08, 0.07
Microwave 15 min high 0.06, 0.05
Microwave 1.5 min high 0.96, 0.43
Microwave 3 min high 1.47,2.73
Microwave 5 min high 0.02, 0.02
migration is either not detectable or barely above the limit of
detection. Slightly higher levels of oligomers were found in
the samples of alcoholic beverages as might be expected for a
more aggressive extraction medium, and the higher surface
area to volume ratio of the miniature bottles which favors
higher migration values. Some differences in replicate results
for individual samples of the same beverage were observed,
reflecting possible differences in storage times and prior
history for these survey samples.
Migration of PET oligomers into olive oil on repeated-use of
PET trays
As PET domestic oven-ware trays sold for conventional
or microwave cooking are intended for repeat-use, it was of
interest to examine the migration behaviour for this applica-
tion. Proposed EC regulations allow for the expected decline
in overall migration from the first to subsequent uses of the
article by accepting the migration value obtained after 3
consecutive tests on the same article using fresh simulant on
each occasion, as that pertaining to the test limit. As it is not
possible to carry out actual overall migration experiments into
olive oil in this fashion on the same article, this approach was
of necessity decided by the Commission on the basis of only
limited supporting experimental data. For PET articles the
oligomer migration gives a good measure of the total migra-
tion from this material and thus successive measurements of
the migration of these species can be used as a basis for
measuring the actual reduction in migration that occurs in
practice on repeat-use.
The results shown in Table 3 for migration experiments
into olive oil were carried out under test conditions of 2 h at
175°C representing an extreme test compared with likely
practical applications. Migration was measured into a rela-
tively small volume of oil and therefore data are expressed in
mg/dm 2 i.e. calculated as loss of oligomers from the tray rather
than as a level of contamination in the oil. Under these test
conditions it can be seen that oligomer migration drops from
an initial level of 1.71 -1.79 mg/dm 2 to 0.34 - 0.35 mg/dm 2
 MIGRATION OF PLASTICS INTO FOOD DURING COOKING 341

TABLE 2. Migration of PET oligomers from PET bottles into beverages

Beverage type Bottle volume No. PET oligomers (mg/kg)*
(ml) samples Mean
Gin 50 2 0.12,0.47 0.29
Rum 50 3 0.06, <0.05, <0.05 <0.05
Vodka 50 3 0.07, 0.14, <0.05 0.08
Whisky 50 2 0.08, 0.08 0.08

Cola 250 3 <0.05, <0.05, <0.05 <0.05

Ginger Ale 500 4 0.08, <0.05, 0.14, 0.06 0.08
Soda water 500 1 <0.05 <0.05
Tonic water 500 1 <0.05 <0.05
Bitter lemon 500 1 0.05 0.05
Limeade 250 1 <0.05 <0.05
*Replicate results for individually purchased samples.

TABLE 3. Migration of PET oligomers from trays into olive oil on Testing of PET trays from different manufacturers for oli-
repeat-use, (migration experiments for 2 h at 175V). gomer migration
Number of successive PET oligomer migration
Tn order to examine whether the type of PET cookware or
exposures (rr g/dm-)
Tray A TrayB the manufacturer would lead to any differences in oligomer
1 1.71 1.79 migration levels, a number of trays from different sources
2 0.86 0.82 were tested with olive oil for 2 h at 175°C. These test condi-
3 0.64 0.51 tions were used for comparative purposes only and were
4 0.53 0.50 accepted as being extreme in relation to normal use. The
5 0.64 0.46 results are shown in Table 4 for duplicate tests of 5 different
Three week resting period
6 0.60 0.51
7 0.49 0.40
8 0.34 0.35 1BL (a )
Mean of tests 1-8 0.72 0.66

m / z 16 3

after 8 successive tests. The three week resting period after test
5 was to examine for re-equilibration of oligomers within the
PET tray i.e. to see whether oligomer diffusion within the
plastic to the surface was becoming rate-limiting on succes- m / z 16 7

sive repeat-use. An effect, although not particularly signifi-

4 . 0 4.5
cant, of this resting period was observed in that oligomer
T i m e (m i n)
levels for test 5 and 6 are about equivalent, prior to a continued
drop in migration on subsequent testing.
The most significant drop in migration was observed in 1BBL, (b)

going from test 1 to test 2, and thereafter a steady reduction SB

BB
was observed. The mean values for oligomer migration are
48
shown in Table 3 calculated on the basis of all 8 test results. m / z 16 3
The result of using test 3 for checking for compliance with the
proposed regulations means that oligomer levels of 0.64 and lBBL
0.51 mg/kg would be the values selected for trays A and B Be
respectively. Tt can be seen that for these PET trays the values ee
obtained by using this third test are in both cases lower than the
mean of 8 successive repeat tests. However, this latter mean m / z 16 7

would be expected to decline as the number of repeat tests was

successively increased. In this particular example the migra-
tion values are far lower than the proposed limit of 10 mg/dm 2 ,
so the choice of the particular test for repeat-use is not critical.
However in other cases where the material is much closer to
the tolerance limit, the basis for selection of the value for
repeat-use could be far more crucial in determining a pass or
failure in the global migration test.
4.0
Time ( m i n )
Figure 1. Selected Jon Monitoring Chromatograms illustrating PET
oligomers in (a) Sample of French fries heated in microwave
susceptor carton (containing 2.73 mg/kg total PET oligomers), (b)
Sample of vodka in an airline PET bottle (containing 0.J 4 mg/kg
total PET oligomers).

JOURNAL OF FOOD PROTECTION. VOL. 52, MAY 1989

342 CASTLE, MAYO, CREWS AND GILBERT

TABLE 4. Migration of PET oligomers from PET trays into olive oil
under test conditions of 2 h at 175 °C.
Cookwater Article PET oligomers
mg/dm2
PET tray (manufacturer A) 1.7, \A
PET tray (manufacturer B) 1.8,1.9
PET airline tray (manufacturer C) 2.0, 2.4
PET airline tray (manufacturer C) 3.8, 4.2
PET coated paperboard (manufacturer D) 1.7, 1.6
types of trays from 4 different m a n u f a c t u r e r s . T h e results in all
cases fall within the r a n g e 1.4 to 4.2 m g / d m 2 and the levels
o b s e r v e d do not appear to be significantly influenced by the
thickness of material w h i c h r a n g e s from a thin film coating on
paperboard to 0.32-0.34 mm thick section for PET trays.
REFERENCES
1. Ashby, R., 1988. Migration from polyethylene terephthalate under all
conditions of use. Food Addit. Contain., 5:485-492.
2. Castle, L., M. Sharman, and J. Gilbert. 1988. Gas chromatographic-mass
spectrometric determination of epoxidized soya bean oil contamination
of foods by migration from plastic packaging. J. Assoc. Off. Anal.
Chem., 71:1183-1186.
3. Castle, L., A. J. Mercer, and J. Gilbert. 1988. Gas chromatographic-mass
spectrometric determination of adipate-based polymeric plasticizers in
foods. J. Assoc. Off. Anal. Chem. 71:394-396.
4. Castle, L., A. J. Mercer, J. R. Startin, and J. Gilbert. 1988. Migration from
plasticized films into foods 3. Migration of phthalate, sebacate, citrate
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JOURNAL OF FOOD PROTECTION, VOL. 52, MAY 1989