TFAC2008 397PrintingInks FromInkstoFood

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Migration of novel offset printing inks from cardboard packaging into food
Article in Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment · September 2009
DOI: 10.1080/19440040903241952 · Source: PubMed
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Food Additives and Contaminants
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Printing Inks: From Inks to Food

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Journal: Food Additives and Contaminants
Manuscript ID: TFAC-2008-397.R1

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Manuscript Type: Original Research Paper
Date Submitted by the

27-Jul-2009
Author:
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Complete List of Authors: Richter, Tina; SQTS - Swiss Quality Testing Services
Gude, Thomas; SQTS - Swiss Quality Testing Services
Simat, Thomas; Technical University of Dresden, Institute of Food
ie
Chemistry, Chair of Food Science and Food Skin Contact Materials
Methods/Techniques: In-house validation, LC/MS

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Additives/Contaminants: Food contact materials, Migration, Packaging paper and board
Food Types: Confectionary, Meat

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http://mc.manuscriptcentral.com/tfac Email: tfac@csl.gov.uk

Page 1 of 17 Food Additives and Contaminants
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Migration from novel offset printing inks from cardboard packaging
5 into foods
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7 Tina Richter1,2, Thomas Gude1, Thomas Simat2
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9 1
Swiss Quality Testing Services (SQTS), Grünaustrasse 23 Dietikon 8953 Switzerland
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Technical University of Dresden (TUD), Institute of Food Chemistry, Dresden, Germany
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15 Abstract
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17 In this paper we report the migration potential of newly patented low-migration offset printing
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19 inks from cardboard food packaging. The purpose was to estimate the potential risk of migra-
20 tion into food. As starting point the complete printing formulation was available. Due to the
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22 fact that the solvent compounds in these inks are different from those used in conventional
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24 printing inks, the investigation was focused on these solvents. Instead of containing mineral
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25 and vegetable oils, the low-migration printing inks are based on novel fatty acid ester. The
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27 migration of this alternative solvent was investigated according to DIN EN 14338 in the simu-
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lant Tenax and in different types of food. For specific detection of the fatty acid ester, the
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30 method chosen was LC-MS/MS (APCI), due to the higher sensitivity and selectivity com-
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32 pared to GC/MS. Printed packaging materials from three different commercially available
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food products (meat, chocolate and sweets) were chosen to be tested. The migration of the
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35 fatty acid ester from the packaging into simulants was demonstrated by analysis. To analyse
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food samples, a clean-up method based on solid phase extraction was developed. The mi-
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38 gration of the fatty acid ester into foods like meat, chocolate and sweets could also be dem-
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40 onstrated. Levels of contamination of these foods were between 5 and 80 µg fatty acid es-
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42 ter/kg. The amounts found in food were lower than the amounts in simulants.
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45 Keywords: printing inks, migration, paper and cardboard, packaging materials, food con-
46 tamination
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52 Introduction
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Printing inks normally consist of four major components – colouring matters (pigments or
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55 dyes), vehicles (resins), solvents (depending on the printing process) and a large number of
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57 additives, but with a low percentage in inks. Inks applied to food packaging materials are not
58 covered by specific European legislation. However, according to Regulation EU
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60 No.1935/2004 materials and articles in contact with food should comply with the general cri-
teria laid down in Article 3 (European Commission, 2004). They should be manufactured in
such way that they do not “transfer their constituents to food in quantities which could en-
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Food Additives and Contaminants Page 2 of 17
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3 danger human health, bring about an unacceptable change in the composition of the food or
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5 bring about deterioration in the organoleptic characteristics thereof.”
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8 The European Printing Ink Association (EuPIA) is planning to set up a “positive” list in the
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10 next five to ten years as an answer to the “ITX case”. This substance hit the headlines in
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September 2005 because the Italian Food Control Authority detected that the ITX (2-
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13 isopropyl thioxanthone) migrated into baby milk at levels up to 250 µg/l (European Commis-
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15 sion, 2005; Nestlè 2005). ITX is used as a photoinitiator in UV cured inks. But these specific
16 measures from EuPIA seem to be far in the future, because national authorities are planning
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18 to implement a positive list in their national food contact material regulations. In April 2008
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Switzerland was the first country that included arrangements for printing inks in its national
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21 regulation on food contact materials (Swiss Regulations, 2008). At the moment there only
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23 exists a notification requirement, based on the Council of Europe Printing Ink Recommenda-
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tions of 2005 (Council of Europe, 2005), which also reiterated the criteria of 1935/2004. This
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26 situation may create a lot of excitement within the printing industry, the packaging industry
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28 and especially in the food industry.
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31 To fulfil food manufacturer’s needs as well as the recently implemented or planned national
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regulations, the printing ink industry developed new low-migration printing inks. The solvent
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34 compound is different from those used in conventional offset printing inks. Instead of contain-
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36 ing mineral and vegetable oil, the newly developed low-migration printing inks are based on
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novel fatty acid ester (short: FAE). The FAE is based on a quaternary alcohol and is esteri-
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39 fied with short fatty acids (more details are confidential). The single compound which have a
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41 higher molecular weight (i.e. 650 Da) is illustrated in Figure 1. Droz & Grob (1997) reported
42 that mineral oil compounds found in cardboard packaging come from printing inks used on
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44 the outer surface of the packaging materials (Droz & Grob, 1997). Especially dry foods, such
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46 as baby foods and cereals are affected. They analysed the contained mineral oil compounds
47 by using on-line coupled LC-GC-FID. The concentrations found in the food ranged from 10 to
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49 150 mg/kg. Besides increasing molecular weight it is possible to introduce reactive or poly-
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meric additives to lower migration (Boon, 2008).
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54 Most paper and cardboard food packaging materials are printed in offset print because it
55 gives a better commercial appeal to the stored product. This is an indirect planographic print-
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57 ing process. The applied ink film is on average 1,5 g/m2 of thickness on one side and dries
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59 by evaporation. For testing the migration of substances from paper and cardboard packaging
60 materials there are several regulations. The EU Directive 82/711/EEC (European Council,
1982) on the basic rules of migration shows a correlation table for the contact conditions for
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3 migration tests and the EU Directive 85/572/EEC (European Council, 1985) contains a list
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5 that indicates which food is represented by which food simulant. Tenax, also known as modi-
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fied polyphenylene oxide (MPPO), is a 'solid' matrix to substitute fat simulant D (olive oil).
8 Tenax is a porous polymer with a large internal surface for high absorption at temperatures
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10 equal to or higher than 100 °C (Jickells & Castle, 1993, Piringer et al.,1993). The DIN EN
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14338 (DIN, 2003) gives the basics for migration tests with Tenax. Paper and cardboard ma-
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13 terials are porous materials with a heterogeneous network of fibres with large air spaces.
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15 Low molecular weight substances from the surrounding air or from packaging material can
16 migrate into the packed food.
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Migration tests with simulants are usually the method of choice. But it is known that migration
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21 tests may overestimate or in some cases underestimate the real levels of migration into food
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23 (Grob & Fankhauser-Noti, 2006). For food manufacturers however it is absolutely important
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to know the residue situation in food, because the results in food prevail. Additionally, certifi-
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26 cation bodies like BRC (British Retail Consortium, 2008) or IFS (International Food Safety,
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28 2007) require testing of packaging ingredients into food. Therefore, it might be useful to ana-
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29 lyse the migration of selected ingredients of printing inks into food to come to a better risk
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31 estimation.
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34 In the present work the results of simulate migration tests were compared with the detected
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36 concentrations in food samples. Meat loaf, chocolate and sweets were selected as matrices
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to cover a complete range of food matrices. For all packaging materials there was no direct
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39 food contact between food and print.
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42 Materials and methods
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45 Samples and materials
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47 The printed cardboard materials to be tested were partly delivered by the manufacturer and
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49 partly bought on the market. The three different samples summarised in Table 1 were very
50 different in composition. The meat packaging was laminated with poly-(1,4-
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52 butylenterephthalate) (PBP) and was delivered by the manufacturer. The two following pack-
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aging materials were bought from commercial market. The food contact surface of the choco-
55 late packaging is printed with black letters, that means inside of the packaging material. And
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57 the packaging of sweets is also coated with a barrier lacquer, whose composite is not known.
58 The food was stored in the tested packaging: meat with 22% fat, chocolate with 39% fat
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60 and a cocoa content of at least 52% and sweets with no fat and only carbohydrates. These
chosen different food types represented food classes with high, middle and no fat content.
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3 The solvents and chemicals were analytical grade and purchased from Merck and Fluka.
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5 The Tenax (TA 60/80 mesh), a porous polymer of polyphenylene oxide with a high molecu-
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7 lar weight, with a very high temperature stability (Tmax = 400 °C), a high surface area and low
8 specific mass (0.23 g/cm3), was purchased from Sigma-Aldrich, Germany. It was cleaned up
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10 prior to use by Soxhlet extraction using high purity diethyl ether. Florisil was used for sample
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preparation and purchased from Fluka. The fatty acid ester was provided from the manufac-
13 turer of the low-migration printing inks.
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16 LC-MS/MS system
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18 An HPLC-system from Agilent Technologies was coupled with a MS/MS-system Quattro from
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20 Micromass. Aliquots of 25 µl were injected into an Agilent Zorbax Eclipse XDB-C8 (4.6 mm x
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21 150 mm, 5 µm) in a 50 °C hot column oven. The mobile phase was acetonitrile A and water
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23 B (incl. 20 mg ammonium acetate and 0.01 % formic acid). The mobile phase was applied in
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gradient mode. Starting gradient was 85 % A (2 min isocratically) rising to 100 % A during 6
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26 min and finally holding for 10 min. The flow rate was 0.6 ml/min. Different columns and dif-
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28 ferent compositions of the mobile phase were investigated in terms of excellent peak detec-
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tion. The ionisation type was the atmospheric pressure chemical ionisation in the positive
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31 mode under MRM (multiple reaction monitoring) conditions. The precursor ion was m/z 641.5
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33 and the product ions were m/z 127 (Dwell time 0.1min, collision energy 40V) and m/z 497
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34 (Dwell time 0.1 min, collision energy 14V). The MS/MS parameters were initially tuned to
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36 FAE to find the optimum settings for the instrument.
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39 Extraction of total packaging materials
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41 To obtain the percentages of fatty acid ester migrate from the absolute content of the pack-
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aging during the migration into the food, the packaging materials were extracted with diethyl
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44 ether on the reflux for 6 hours. The diethyl ether was evaporated in a closed system by recy-
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46 cling the solvent. The residue was dissolved with 10 ml acetonitrile and was analysed by LC-
47 MS/MS.
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Migration experiments from packaging materials
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52 The migration conditions applied in the migration experiments were selected according to
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54 normal use of the packaging and the EU Directive 82/711/EEC (European Council 1982)
55 (see first line in Table 2). The test medium was Tenax.
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57
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59 Migration tests using Tenax as adsorbent. The experiment has been carried out according to
60 DIN EN 14338 [12]. Below the method is explain briefly. The quantity of Tenax needed for
the migration was in each case calculated according to the prescribed ratio of 4g Tenax/dm2.
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3 In the experiment the Tenax amount was filled into the bigger part of a Petri dish and spread
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5 evenly over the bottom. Then a circulare shape of 1dm2 was cut from the printed substrate.
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The food contact surface of the cardboard was placed into the Petri dish on the Tenax and
8 closed with the other part of the Petri dish. After exposure time the cardboard was removed
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10 and the Tenax was extracted with diethyl ether. To determine the overall migration the ether
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extract was evaporated to dryness in a closed system by recycling the solvent. The overall
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13 migration was determined by weighing the non-volatile residue. After weighing the residue,
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15 including the fatty acid ester, it was carefully dissolved with 10 ml acetonitrile. The solution
16 was ready for LC-MS/MS to determine the specific migration of fatty acid ester.
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Sample preparation
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21 To analyse the fatty acid ester in the presence of the matrices of meat, chocolate and sweets
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23 it was necessary to develop a new method for the separation of the analyte. The difficulty of
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this problem was that the recovery rates of liquid-liquid extraction such, as extraction with
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26 hexane, are very low. Hexane is very non-polar and thus not suitable to extract the fatty acid
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28 ester. So a new method for this substance had to be developed. For the validation of the
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29 method the three used matrices were from the same type of later analysed foodstuff but not
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31 out of this researched packaging. The food stuffs were also analyzed previously to be free
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from possible contaminations prior to its use in this part of this study.
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36 At first 5 g of food was extracted (1 min) with 50 ml of a 1:1 (v/v) mixture of cyclohexane/ethyl
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acetate with a high-speed mixer. A spoonful of sodium chloride was added during the extrac-
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39 tion for better phase separation. The solution was centrifuged at 3000 rpm for 5 min. 1 ml of
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41 the supernatant was evaporated under nitrogen to dryness and reabsorbed with 1 ml hex-
42 ane. To separate the substances from the matrices the extract was poured over a solid
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44 phase of 2 g of Florisil with 2 g of sodium sulphate (1g over and 1g under the Florisil bed).
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46 The cartridge was previously conditioned with 5 ml hexane. Then the fatty acid ester was
47 eluted with 15 ml 1:1 (v/v) mixture of diethyl ether/hexane. The resulting eluate was blown
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49 dry with nitrogen and reconstituted with 1 ml acetonitrile. The solution was filtrated by mem-
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brane filter (0.45 µm) and chromatographic analysis was carried out.
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52
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54 During development of this method the different steps of the sample preparation were exam-
55 ined. The second extraction step with SPE was necessary because of the low recoveries
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57 after the first extraction with cyclohexane/ethyl acetate. The validation of this procedure was
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59 arranged with three different levels of fortification (10µg/kg, 100µg/kg and 1000µg/kg food)
60 and on two different days, in each case with a fivefold determination. Control samples were
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3 not fortified. The recoveries for the complete sample preparation were >70% for all three ma-
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5 trices for all three fortification levels. The results of this examination are listed in Table 3.
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8 Results and discussion
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10 Chromatography methods
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12 The combination of LC with tandem mass spectrometry ensures a high level of specificity. A
13 two stage selected ion recording could be performed by using multiple-reaction monitoring
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15 (MRM), which increased the selectivity. This detection mode and the comparisons with the
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respective retention times allowed the FAE to be identified and quantified.
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20 The limit of detection (LoD) for the analyte was 0.07 µg/l and the limit of quantification (LoQ)
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21 was 0.2 µg/l. A typical chromatogram of a standard solution at the LoQ is shown in Figure 2.
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Calibration was performed using external standards in the concentration range of 0.25 µg/l to
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26 150 µg/l. The compound showed linear correlation between signal area and concentration
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28 with 10 calibration points.
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31 Overall migration of packaging materials
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33 The gravimetrically identified overall migration with Tenax from all the analysed cardboard
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34 packaging materials was below 1 mg/dm2. The conditions of migration are given in Table 2
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36 (first line).
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39 Total extract of fatty acid ester and specific migration in packaging materials
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41 The other results given in Table 2, show that the specific migration of the FAE with Tenax
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was less than 0.5 % (even less than 0.1 %) from total content of the whole packaging mate-
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44 rial. The translation from µg/dm2 into µg/kg was done using the real relationship between
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46 packed food and surface area and not with the known conversion factor of six (European
47 Commission, 2002). The high factors are based on the very small portion in big packaging.
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51 Validation of the method
52 The validity of the complete sample preparation method was investigated by performing re-
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54 covery experiments. Control foodstuffs were fortified at three different fortification levels. The
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values obtained for the whole process (SPE and quantification procedure) have RSD < 20 %
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57 based on five replicates on two different days (see Table 3).
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60 Based on the validation results the lowest concentration yielding acceptable accuracy (74-
103 %) and precision values (< 20 %) was selected as Limit of quantification (LoQ = 10
6
1
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3 µg/kg). The limit of detection was graphically determined by the signal to noise ratio greater
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5 than 3 (LoD = 3 µg/kg). Figure 3 shows the chromatogram of 10 µg/kg spiked concentration
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of the matrix chocolate by LC-MS/MS. The retention time is 13,65 min in the multiple reaction
8 monitoring modus (MRM-Mode).
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Analysis of food samples
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13 The food samples were bought in commercial markets in Switzerland and were analysed
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15 after sample preparation as previously described. Migration of FAE into foods occurred in all
16 three samples with values ranging between 5 to 80 µg/kg. The packed meat loaf and choco-
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18 late was analysed three times in duplicate (meat loaf: 16.9 – 23.1 µg/kg, chocolate: 7.7 –
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35.4 µg/kg). The quantification of FAE in the packed sweets was analysed five times in dupli-
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21 cate (20.1 – 78.8 µg/kg). The average values are shown in Figure 4. Reagent blanks and
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23 sample blanks were also analysed for strict standards of zero background contamination of
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FAE.
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28 Although no direct food contact existed, on average a low amount of FAE was detectable in
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29 all matrices. These residues may be traced back to permeation. The meat loaf was in the
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31 oven at a high temperature for more than an hour, but not covered. The chocolate and the
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sweets were stored closed, so that out-gassing from packaging material into food might be
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34 responsible. Another reason is the phenomenon of set-off during the storage time in the
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36 manufactures. Stacking the sheets of printed food packaging materials one on the top of the
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other is common in such packaging premises. Set-off is the unwanted transfer of molecules
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39 from the printed surface of food packaging materials to the interior non-printed surface in
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41 stacks or roles.
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44 The high amount in sweets in comparison to the two other matrices may be attributed to the
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46 bigger surface of the cubical single pieces in the package and the longer best before date.
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49 Specific migration in packaging materials and foods – a comparison
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The concentration of the fatty acid ester found in packaging materials and in food differed by
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52 factor 4 to 9 (see Figure 4). Therefore, the simulations do overestimate the real values in
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54 food. But if you take the reduction factor of EU 85/572/EEC as a basis for a new calculation,
55 the simulation tests perform approximately the same values as in food. Only for meat loaf a
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57 factor of 2 is observed. For some types of food in combination with a fatty simulant a reduc-
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59 tion factor is necessary because of higher extraction efficiency. For meat the reduction factor
60 (RF) is four, for chocolate five and for sweets also four. By utilising the reduction factor a
good prediction for the specific migration of FAE with simulants is possible. But questionable
7
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3 is if this reduction factor is to the extent to which they may be applicable. One fact is, that the
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5 reduction factor is only relevant for the overall migration values. Another fact is that the FAE
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is not listed in the EU Directives 2007/19/EC annex IVa (European Commission, 2007). So
8 the proposed fat reduction factor (FRF) for lipophilic substances which shall correct the spe-
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10 cific migration of foods containing more than 20 % fat is not relevant. The specific migration
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of lipophilic substances shall be corrected by the FRF variable between 1 and 5.
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15 Without consideration of the reduction factor the described results show clearly that simula-
16 tion tests are typically not sufficient to perform a real risk estimation. Typically food manufac-
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18 tures get results from simulation tests on the basis of which they have to decide whether to
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take the packaging for the intended use or not. Due to the fact that simulation might over- or
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21 underestimated, the real situation is not known. In the described case we found an overesti-
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23 mation for all three matrices. The low values found in food are much better for the food
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manufacturer than the simulation values.
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28 From these values it becomes clear that food manufacturers need more information regard-
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29 ing the printing ink ingredients. Without this knowledge only simulation tests can be used for
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31 decision making, which is not in all cases the best.
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34 Conclusions
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36 In this study new patented low-migration printing inks were tested for migration of included
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38 substances. The fatty acid ester (FAE), which was chosen as a kind of marker substance,
39 migrates from the material into the food over the gas phase, because there are no contact
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41 between the food and the print of the packaging material. This method has been shown to be
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suitable for detecting low levels of FAE in different matrices.
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46 The risk of residual printing ingredients might be negligible for the investigated substance,
47 because all values are around 50 µg/kg or below (as mean value), which is the limit set by
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49 the EuPIA guideline for moderate toxicologically characterized substances.
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52 Finally, for good risk estimations in food leading to full risk assessments it is mandatory that
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54 food manufacturers have access to complete information on formulations. Otherwise migra-
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tion simulations will be taken with the risk of over- and underestimation and do not show the
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57 real situation in food.
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References
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8
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10 Boon, A. (2008) Migration from food packaging inks – issues & some solutions. Oral presen-
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12 tation presented at ILSI conference 19 – 21 November 2008, Prague, CZ.
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15 British Retail Consortium (2008) BRC/IoP Global Standard – British retail consortium, Ver-
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sion 3 (2008)
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20 Council of Europe (2005), Council of Europe, Committee of Ministers, Resolution AP (2005)
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21 2 on packaging inks applied to the non-food contact surface of food packaging materials and
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23 articles intended to come into contact with foodstuffs, document available at
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http://www.coe.int/t/e/social_cohesion/soc-sp/public_health/food_contact/presentation.asp
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28 DIN (2003), DIN EN 14338:2003, Papier und Pappe vorgesehen für den Kontakt mit
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Lebensmitteln – Voraussetzung für die Bestimmung des Übergangs von Papier und Pappe
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31 durch Anwendung von modifizierten Polyphenylenoxiden (MPPO) als ein Simulanz.
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33 Schweizer Norm: 2004-09
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36 Droz C, & Grob K. (1997). Determination of food contamination by mineral oil material from
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38 printed cardboard using on-line coupled LC-GC-FID. Z. Lebensm. Unters. Forsch. 205: 239-
39 241.
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European Commission (2002), EU Commission Directive 2002/72/EC relating to plastics ma-
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44 terials and articles intended to come into contact with foodstuff of 6 August 2002
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49 and of the council on materials and articles intended to come into contact with food and re-
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51 pealing Directives 80/590/EEC and 89/109/EEC of 27 October 2004
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54 European Commission (2005), The Rapid Alert System for Food and Feed (RASFF), Annual
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Report 2005, document available at
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57 http://ec.europa.eu/food/food/rapidalert/report2005_en.pdf
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60 European Commission (2007) Commission Directive 2007/19/EC amending Directive
2002/72/EC relating to plastic materials and articles intended to come into contact with food
9
1
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3 and Council Directive 85/572/EEC laying down the list of simulants to be used for testing
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5 migration of constituents of plastic materials and articles intended to come into contact with
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foodstuffs of 30 March 2007
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10 European Council (1982), EU 82/711/EEC Council directive laying down the basic rules nec-
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essary for testing migration of the constituents of plastic materials and articles intended to
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13 come into contact with foodstuffs of 18 October 1982
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16 European Council (1985), EU 85/572/EEC Council directive laying down the list of simulants
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18 to be used for testing migration of constituents of plastic materials and articles intended to
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come into contact with foodstuffs of 19 December 1985
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23 Grob K, & Fankhauser-Noti A. (2006). Migration of plasticizers from plastisol gaskets of lids
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for glass jars into oily foods: gasket material in food contact, proportion of plasticizer migrat-
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26 ing into food, testing by simulation. Trends in Food Science & Technology. Vol. 17: 105-112
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28
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29 International Food Safety (2007) IFS – International Food Safety, Version 5 (2007)
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Jickells S & Castle L. (1993). Combined compositional analysis and threshold of regulation
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34 as a possible control measure for microwaves susceptors. Food Additives and Contami-
35
36 nants. 10: 647-653
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39 Nestle (2005), Chronology of withdrawal of Nestlè and other liquid milks, document available
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41 at http://www.ibfan.org/site2005/abm/paginas/articles/arch_art/416-1.doc
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44 Piringer O-G, Wolff E & Pfaff K (1993). Use of high temperature-resistant sorbents as simu-
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46 lants for testing. Food Additives and Contaminants. 10: 621-629
47
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49 Swiss Regulation (2008), CH-Regulation on food contact materials (Eidgenössisches Depar-
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tement für Inneres), cited 23.11.2008 in version from 01.04.2008
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15 Figure 1: novel fatty acid ester (FAE)
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5 100
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22 0
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24 Figure 2: LC-MS/MS-chromatogram of standard solution (0,2 µg/l FAE) in acetonitrile (tR =
ee
25 13,65 min).
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0 Time
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24 Figure 3: LC-MS/MS-chromatogram of a chocolate sample fortified with FAE (tR = 13,65 min).
ee
25 The concentration level is 10 µg/kg.

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Figure 4: Concentration of specific migration fatty acid ester in Tenax (left: without reduction
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26 factor (RF), right: with reduction factor (RF) of EU 85/572/EEC) and in food in µg/kg.
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3 Table 1: Details of cardboard samples
4
Test Sample Supplier code Ink, print substrate
5
6 Packaging for meat loaf A low-migration offset printing inks,
2
7 board with 250 g/m grammage
8 Packaging for chocolate B low-migration offset printing inks,
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9 board with 300 g/m grammage
10 Packaging for sweets C low-migration offset printing inks,
11 unknown
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4 Table 2: Conditions and results of migration experiments
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Packaging for Packaging for Packaging for
6
7 meat loaf chocolate sweets
8 Migration conditions (according to
9 70 min at 150 °C 10 d at 40 °C 10 d at 40 °C
10 description on packaging material)
11 Overall migration [mg/kg] <1 <1 <1
12 Absolute content of FAE in packaging
13 2 7500 6400 7200
14 materials [µg/dm ]
15 Specific migration of FAE
2 Tenax: 23.7 Tenax: 1.9 Tenax: 5.1
16 from packaging materials [µg/dm ]
Fo
17
relate to % of total content Tenax: 0.32 Tenax: 0.03 Tenax: 0.07
18
19 Specific migration of FAE
Tenax: 174.3 Tenax: 87.4 Tenax: 199.6
20 Conversion in µg/kg
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5 Table 3: Results of the sample preparation validation
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Mean of day one and day two 10 µg/kg 100 µg/kg 1000 µg/kg
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8 meat loaf:
9 recovery rates in % 102.5 104.9 87.6
10 standard deviation in µg/kg 1.6 10.8 59.9
11 relative standard deviation in % 15.6 10.3 6.8
12 chocolate:
16 sweets:
Fo

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TFAC2008 397PrintingInks FromInkstoFood

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Tina Richter Thomas Gude

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Thomas Joachim Simat

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Printing Inks: From Inks to Food

Journal: Food Additives and Contaminants

Manuscript ID: TFAC-2008-397.R1

Manuscript Type: Original Research Paper

Date Submitted by the

Chemistry, Chair of Food Science and Food Skin Contact Materials

Methods/Techniques: In-house validation, LC/MS

Additives/Contaminants: Food contact materials, Migration, Packaging paper and board

Food Types: Confectionary, Meat

http://mc.manuscriptcentral.com/tfac Email: tfac@csl.gov.uk

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http://mc.manuscriptcentral.com/tfac Email: tfac@csl.gov.uk

25 The concentration level is 10 µg/kg.

http://mc.manuscriptcentral.com/tfac Email: tfac@csl.gov.uk

http://mc.manuscriptcentral.com/tfac Email: tfac@csl.gov.uk

http://mc.manuscriptcentral.com/tfac Email: tfac@csl.gov.uk

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17 recovery rates in % 74.1 109.1 101.7

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