Evolving Food Packaging Regulations in Korea and Migration Testing with Tenax

Transcription

1 2017 Food Contact Material Safety Symposium (Xian, China) 02. Nov Evolving Food Packaging Regulations in Korea and Migration Testing with Tenax Keun Taik Lee Dept. of Food Processing and Distribution Gangneung-Wonju Nat. Univ., Rep. of Korea Tel : , leekt@gwnu.ac.kr

2 O u t l i n e 1. Regulatory entities and safety control system 2. Current regulations, specifications and standards for FCMs 3. Progress in the FCMs regulations 4. Issues related to FCMs 5. Needs of global harmonization in the migration testing methods 6. Migration testing with Tenax 7. Conclusions

3 Restructuring History of Regulatory Bodies for FCMs 1 April 1996 Feb June 2002 April 2009 Mar : The Korea Food and Drug Safety Headquarter was founded. Containers and Packages Division started its duty. : The Korea Food and Drug Safety Headquarter was elevated in status to an Administration (Korea Food and Drug Administr.; KFDA). : The National Center of Toxicological Research was reorganized to the National Institute of Toxicological Research. : The National Institute of Toxicological Research was transformed into the National Institute of Food and Drug Safety Evaluation (NIFDS). : Min. of Food and Drug Safety (MFDS) was elevated in status from KFDA.

4 Governmental Safety Control System for FCMs 2 Inquiry MFDS Local authorities (Provinces, Counties, Cities etc.) Response to the inquiries from public or industries Notice Legal actions against violation Inquiry Report NIFDS Safety evaluation Risk assessment Research

5 Food Sanitation Act (FSA) 3 Jan Apr Enacted by Act No Standards and Specifications for FCMs including plastics, metals, ceramics, and feeding apparatus were established. (Ordinance 249, Min. of Health and Social Affairs) (Initially for 9 kinds of FCMs)

6 Food Sanitation Act (FSA) 4 I III IV V VI Chapter I General Provisions Chapter III Apparatus, containers, and packages Chapter IV Labels Chapter V Food Code Chapter VI Inspection etc. Article 1. Purpose Article 2. Definitions Article 8. Prohibitions of Sale and Use of Poisonous Apparatus etc. Article 9. Standards and Specifications Article 10. Criteria for Labels Article 14. Food Code etc. Article 19. Report of Imported Foods, etc. Article 31. Mandatory Self-Quality Inspection

7 Food Sanitation Act ; Article 19 Inspection of Domestic and Imported Food-Contact Utensils, Containers and Packages Presently in Korea, FCAs are not controlled by a pre-market approval system like the positive list system. FCMs are not assessed on the basis of the raw materials used, but on the basis of the finished product s performance in material and migration tests. Domestic goods : should be tested according to the Self-Quality Inspection Standard at least once every six months for the same material. (Enforcement Rule of FSA, Article 31, Appendix 12) Imported goods : are closely controlled/inspected before, at the time of import declaration, and thereafter (Special Law for the Safety Control of Imported Foods ; ) Distributed goods in the market : - Domestic goods : Removal inspection either periodically or for special reasons (Enforcement Rule of FSA, Article 20) - Imported goods: Controlled during distribution (Ch. 5, Article 23-26) 5

8 Food Sanitation Act (FSA) 6 Provisional Approval of the Standards and Specifications (FSA Ch. 3, Art. 9, Pg. 2 2 ) Pre-market approval for the FCSs not covered by current regulations Application documents shall include; 1) Name and contact information for the manufacturer of the material 2) Product name 3) Identification of the chemical name for the product 4) Description for the manufacturing process and the intended use 5) Material and migration specifications 6) Test methods used to ensure compliance with these specifications (together with tox. data) Review and decision for the approval within 14 days after submission of documents. The provisional approval may be proceeded until the relevant proclamation shall be appended to the Food Code.

9 7 Standards and Specifications for Food Utensils, Containers and Packages

10 8 English Website for the Standards and Specifications for FCMs in Korea 089

11 9 Standards and Specifications for Food Utensils, Containers and Packages I. General rules II. Common standards and specifications III. Specifications for individual materials IV. Test methods

12 Standards and Specifications for Food Utensils, Containers and Packages II. Common specifications and standards 1. Common manufacturing standards 4) Metals being used for the manufacture or repair of the contact parts of FCAs with foods shall not contain more than 0.1% Pb and 5% Sb. 5) Solders being used for the manufacture or repair shall not contain more than 0.1%. 6) Printing ink : Benzophenone 0.6 mg/l, Toluene 2 mg/m 2 8) FCMs being used for plastics, cellophane, paper, starch shall not contain more than 100 mg/kg (in total) Pb, Cd, Hg, and Cr ) Prohibit the use of DEHP in manufacturing FCAs, except where no migration into foods is possible. 10

13 11 Standards and Specifications for Food Utensils, Containers and Packages II. Common specifications and standards 3. Specifications by material 1) Prohibits the use of DEHA in wrap film (except where no migration into food is possible). 2) Prohibits the use of DBP and BBP in baby bottles and soothers

14 Standards and Specifications for Food Utensils, Containers and Packages III. Specifications by material Plastics (40 in total) Cellophanes : Regenerated cellulose film product Rubbers Papers and Processed papers Metals Wood Glass, Ceramics, Enamels and Potteries Starch Products 12

15 13 Standards and Specifications for Food Utensils, Containers and Packages III. Specifications by material 1. Definition 2. Residue specification (mg/kg) Heavy metals, monomer, limit value, negative list 3. Migrant specification (mg/l) Pb, overall migration, KMnO 4 consumption etc. 4. Testing methods :

16 Standards and Specifications for Food Utensils, Containers and Packages Polyvinylchloride (PVC) Polyethylene (PE), Polypropylene (PP) Polystyrene (PS) Polychlorovinylidene (PVDC) Polyethyleneterephthalate (PET) Phenolformaldehyde (PF) Melamineformaldehyde (MF) Ureaformaldehyde (UF) Polyacetal (POM) Acryl resin Plastics Nylon (PA) Polymethylpentene (PMP) Polycarbonate (PC) Polyvinyl alcohol (PVA) Polyurethane (PU) Polybutene-1 (PB-1) Acrylonitrile-styrene (AS) Acrylonitrile-butadiene-styrene (ABS) Polymethacrylstyrene (MS) Polybutylene terephthalate (PBT) 14 - To be continued

17 15 Standards and Specifications for Food Utensils, Containers and Packages 20 Polyarylsulfone (PASF) 30 Epoxy resin Polyarylate (PAR) Hydroxybutyl polyester (HBP) Polyacrylonitrile (PAN) Fluoro resins (FR) Polyphenylene ether (PPE) Ionomeric resin Ethylene vinyl acetate (EVA) Methylmethacrylate-acrylonitrile-butadienestyrene (MABS) Polyethylene naphthalate(pen) Plastics 31 Polyphenylene sulfide (PPS) Polyethersulfone (PES) Polycyclohexane-1,4-dimethylterphthalate (PCT) Polyimide (PI) Polyetheretherketone (PEEK) Polylactide (PLA) 37 Polybutylene succinate-co-adipate (PBSA) 38 Cross-linked polyester resin

18 16 Standards and Specifications for Food Utensils, Containers and Packages IV. Test methods (Heavy) Metals Lead Cadmium Mercury Hexavalent chromium (Cr +6 ) Antimony Arsenic Barium Germanium Chrome Nickel Barium Zinc etc. Monomers Vinyl chloride Vinylidene chloride Styrene Phenol Formaldehyde Melamine Methylmethacrylate Caprolactam Bisphenol-A Isocyanate Acrylonitrile Diphenyl carbonate Tere- and isophthalic acid etc. Additives etc. DEHP DEHA PCBs Fluorescence whitening agent Toluene BADGE, BFDGE Dibutyl tin Cresol phosphoric acid ester Amines etc.

19 Standards and Specifications for Food Utensils, Containers and Packages Residue specification (Plastics) Type of plastic Acrylic PVC PE/ PP PS PVDC PET PF MF UF POM Details Resin (1) Pb, Cd, Hg, Cr +6 1) (2) Vinyl chloride (3) Dibutyl tin compounds (as DBTD) (4) Cresol phosphoric esters 1, (5) Volatile substances 1) (including styrene, toluene, ethylbenzene, - - 5, isopropyl benzene and n-propyl benzene) (6) Vinylidene chloride (7) Barium (8) BPA (including phenol, bisphenol A and p-t-butyl phenol) (9) Amines(triethyl amine and tributyl amine) (10) 1,3-Butadiene ) As a sum 17 Unit : mg/kg

20 18 Standards and Specifications for Food Utensils, Containers and Packages Migrant specification (Plastics) Unit : mg/l Type of plastic Acryl PVC PE/PP PS PVDC PET PF MF UF POM Details resin (1) Pb (2) KMnO 4 consumption (3) Overall Migration 30 1) 30 2) 30 3) (4) Dibutyl phthalate (5) Benzylbutyl phthalate (6) Di-(2-ethylhexyl) phthalate (7) Di-n-octyl phthalate (8) Diisononyl phthalate (9) Diisodecyl phthalate (10) Di-(2-ethylhexyl) adipate (11) 1-Hexene - 3(PE) (12) 1-Octene - 15(PE) (13) Ba (14) Sb (15) Ge (16) Terephthalic acid (17) Iso-phthalic acid (18) Acetaldehyde (19) Phenol (20) Formaldehyde (21) Melamine (22) Methylmethacrylate ) 1) 150 when n-heptane is used as a food simulant, 2) 150 when use temp. is 100 and n-heptane is used as a food simulant, 3) 240 when n-heptane is used as a food simulant, 4) Limited to the polymers containing 50% MMA within the base polymer

21 Hot Issues on the Safety of Migrated Substances from FCMs DIDP from bottle cap 2006 Colorants and hydrocarbons (C14 ~ C32) from onion net sack 2008 Bisphenol A from baby bottle 2010 Heavy metal from food basin made from recycled plastics 2010 Fluorescent whitening agent from inner paper for chicken packages 2010 Fluorescent whitening agent from pizza box

22 Hot Issues on the Safety of Migrated Substances from FCMs Heavy metals from food packaging paper 2012 Formaldehyde from imported Chinese kitchen wares 2013 Aluminum migration from Al foil 2015 Phthalates from PVC linoleum used for salt ponds 2015 PFCs from frying pan and paper tray Bisphenol A from canned products

23 Safety Assurance Regulations for FCMs 21 General safety only :some South American and Asian countries and certain individual EU countries (only for some FCSs) Licensing/Registration : Argentina, Brazil (for recycled plastics), some Eastern European countries Mandatory Positive Lists : EU, MERCOSUR(BR, AR, PY, UY,VE), China, India, Indonesia, U.S. (if not exempt) etc. Voluntary Positive Lists : Japan, Germany, UK No Objection Letters or Letters of Opinion : Canada, U.S. (for recycled plastics) Combinations of the above many countries/jurisdictions have a combination of requirements in place U.S. is an example. (Baughan, 2006; Ariosti, 2011)

24 PL for FCMs in Canada 22

25 PL for FCMs in Japan 23

26 24 The most critical distinction in FCM regulation systems between countries - Legal stipulation and practical application of a positive list system Presently in Korea, FCMs are not supervised by a premarket approval system like the positive list system. Current Status and Challenges for the Reformation of FCMs Regulations in Korea Positive List System FCMs or FCAs are assessed on the basis of their performance in material and migration tests of finished products. The safety of FCMs and FCAs is evaluated on the basis of whether or not they comply with the general prescription for use condition and with material and migration tests - not by the exposure assessment of the FCSs contained in the material.

27 Merits and Demerits of Korean FCM Regulations 1. Merits Simpler and easier than the positive list system in terms of administration and market surveillance. 2. Demerits Personnel requirements and budget burden Only the manufacturer knows the composition and the amounts of additives in FCMs. It is not practically feasible for the MFDS to identify all substances used to manufacture FCMs or FCAs. Even if goods contain FCSs unapproved by the EU or US positive lists, under the current Korean system, it is rarely feasible to impose sanctions against them if they are unrestricted in Korea. 25

28 Opinions and Call for the Implementation of a PL System for the FCMs in Korea 26 Required stricter control system for FCMs The PL is stricter than the NL for consumer protection The Korea Food Medical News Increased necessity for implementing a positive list system Status and suggestion for the safety control system of FCMs

29 JTBC News on 03. Mar Insecure FCMs No pre-market controls for the FCMs in Korea Positive list systems in the USA, EU and China

30 Factors that Influence Global Products Trade Varying regulatory schemes and data requirements applicable to FCMs Non-tariff trade barrier Lack of global harmonization in terms of specifications and testing methods Compliance testing and relevant documents required for the exported goods 28 (Baughan, 2006)

31 29 Discrepancies in the Migration Testing Methods and Regulations Preparation procedures of tested sample Type of food simulants Testing conditions : temp. and time Migration cell Limit values

32 Migration Testing Conditions and Specifications Country Korea EU USA Source For general use (use at temperature 100 ) For the use at high temperature (use at temperature >100 ) Classification of food types Std. & Spec. for FCMs Simple (70 /30 min or 25 /1 h etc.) Simple (100 /30 min) 4 types EU Reg. 10/2011 CEN, EN Very diverse and specified Very diverse and specified 6 types consisting of 83 different food descriptions Simulants/film area 2 ml/cm 2 1 ml/cm 2 (single side) 0.5 ml/cm 2 (double side) Extraction methods Drying methods RF when using fatty food simulant Limitation of OMVs Total immersion filling article, single side contact using migration cell On hot plate after evaporation Total immersion (double), Tice cell (single), standard pouch(single), filling article (single) etc. On hot plate after evaporation or distillation FAP Simple (121 /2 h or 66 /2 h) Diverse and specified FCN Simple (121 /2 h or 71 /2 h) 10 types 4 types 10 ml/ in 2 (1.55 ml/cm 2 ) Total immersion, filling article, single or double side contact using migration cell etc. On hot plate after evaporation Generally, <30 mg/l, except when using n-heptane as a simulant 10 mg/dm 2 film 60 mg/kg food or simulant 30 Different depending on material type -

33 Recommended Food Simulants Recommended simulants USA Japan Aqueous Acidic Alcoholic Fatty Dry EU 10% ethanol 3% acetic acid 20% 3) or 50% 4) ethanol Veg. oil FAP 1) Dist. water Dist. water or 3% acetic acid FCN 2) 10% ethanol 10% ethanol 10% or 50% 6) ethanol MPPO (Tenax) 8% or 50% 5) ethanol n-heptane None Food oil, HB307, Miglyol 812 Korea Dist. water 4% acetic acid 20% or 50% 6) ethanol n-heptane None MHLW Dist. water 4% acetic acid 20% ethanol n-heptane None PO Dist. water 4% acetic acid 20% ethanol Veg. oil or n-heptane None PVC Dist. water 4% acetic acid 20% ethanol PVDC Dist. water 3% acetic acid 10% ethanol 7) Veg. oil or 95% ethanol, or n-heptane Olive oil or 95% ethanol 1) Food additives petition 2) Food contact notification. 3) For alcoholic foods with an alcohol content of up to 20% and those foods containing a relevant amount of org. ingredients that render the food more lipophilic. 4) For foods containing more than 20% alcohol and for O/W emulsions. 5) For foods containing more than 8% alcohol, 6) Actual ethanol concentration may be substituted. 7) Actual alcoholic strength of the food when it exceeds 10%. 31 None None None

34 Migration Testing Conditions and Simulants for Different Food Types - I Food type Aqueous Acidic USA Japan USA Country Test conditions for the foods stored or heated at 5 20 <T EU >5 /10 d or longer >40 /10 d or longer 70 /2 h or 100 /4 h 100 /1 h or at reflux or 100 /4 h FAP 1) 21 /2 d 49 /1 d Fill boiling /2 h FCN 2) 20 /10 d 40 / 10 d 100 /30 min 40 /10 d 100 / 2 h Korea 70 /30 min 70 /30 min 70 /30 min 100 /30 min EU MHLW 60 /30 min 60 /30 min 60 /30 min 95 /30 min PO 40 /10 d 60 /1 h 90 /30 min 110 /10 min or at bp/90 min PVC 40 /10 d 70 /2 h 100 /30 min 110 /10 min PVDC 40 /10 d 70 /2 h 100 /1 h 121 /1 h Same as with aqueous simulant FAP 21 /2 d 49 /1 d Fill boiling /2 h FCN 20 /10 d 40 / 10 d 100 /30 min 40 /10 d 100 / 2 h Korea 70 /30 min 70 /30min 70 /30 min 100 /30 min MHLW 60 /30 min 60 /30 min 60 /30 min 95 /30 min Japan PO 40 /10 d 60 /1 h 90 /30 min 110 /10 min or At bp/90 min PVC 40 /10 d 70 /2 h 100 /30 min 110 /10 min PVDC 40 /10 d 70 /2 h 100 /1 h 121 /1 h 1,2) Refer to the previous Table (Food simulants). 32

35 Migration Testing Conditions and Simulants for Different Food Types - II Food type Alcoholic Fatty USA Japan USA Country EU Test conditions for the foods stored or heated at 5 20 <T Same as with aqueous simulant FAP 1) 21 /2 d 49 /1 d - - FCN 2) 20 /10 d 40 / 10 d 100 /30 min 40 /10 d 100 (or 71 )/2 h Korea 70 /30 min 70 /30 min 70 /30 min - EU MHLW 60 /30 min 60 /30 min 60 /30 min 60 /30 min PO 40 /10 d 60 /1 h 90 /30 min 110 /10 min or at bp/90 min PVC 40 /10 d 70 /2 h 100 /30 min 110 /10 min PVDC 40 /10 d 70 /2 h 100 /1 h 121 /1 h Same as with aqueous simulant 100 /2 h or at reflux or 121 /1 h or 175 /2 h FAP 21 /30 min 21 /30 min 49 /150 min 66 /2 h FCN 20 /10 d 40 / 10 d 100 /30 min 40 /10 d 100 / 2 h Korea 25 /1 h 25 /1 h 25 /1 h 25 /1 h MHLW 25 /1 h 25 /1 h 25 /1 h 25 /1 h Japan PO 40 /10 d 60 /1 h 90 /30 min 110 /10 min or at bp/90 min PVC 40 /10 d 70 /2 h 100 /30 min 110 /10 min PVDC 40 /10 d 70 /2 h 100 /1 h 121 /1 h 1,2) Refer to the previous Table (Food simulants). 33

36 OMVs into Fatty Food Simulants (mg/dm 2 ) Polymer Thickness ( μm ) n-heptane Iso-octane Soybean oil 95% Ethanol Asia USA EU EU EU EU, USA 25 /60 min 21 / 30 min 40 / 24 h 20 / 48 hr 40 / 10 d 40 / 10 d LDPE LLDPE CPP OPP PET OPA CPA HIPS (79.2 mg/l) GPPS-MPB (126.5 mg/l) HIPS/EPS 200/ PVC PP PVC wrap (102.5 mg/l) (77.5 mg/l) LLDPE wrap (Lee et al., 2002) 34

37 Definition of Food Types according to the Migration Testing Methods of EU, USA, and Japan or Korea 35 Food type EU Type of Simulants USA FAP 1) FCN 2) Japan Korea Aqueous ph>4.5 ph>5.0-3) ph>5.0 ph>5.0 Acidic ph 4.5 ph ph 5.0 ph 5.0 Alcoholic >6% Fatty Classified by the description of food type 4) Those containing alcohol Those containing fat 1,2) Refer to the previous Table (Food simulants). 3) Categorized as defined in 21 CFR (c) Table 1, 4) The criteria of fat content for fatty food is not established, but the fat content of tested food is being considered by applying different reduction factor. x Not defined - 1% x - 20% x

38 Substances Regulated in the EU or Korea (detected from a retort pouch composed of PET/Al/PA/CPP) Substance Use as monomer or other starting substance or macromolecule obtained from microbial fermentation (PPA) Use as monomer or other starting substance or macromolecule obtained from microbial fermentation Caprolactam YES YES Butylated hydroxytoluene (BHT) Tris(2,4-di-tertbutylphenyl )phosphate (lrgafos 168) Octadecyl 3-(3,5-di-tert- butyl-4- hydroxyphenyl)propionate (Irganox 1076) 1-Isocyanato-3- isocyanatomethyl-3,5,5- trimethylcyclohexane YES NO EU SML (mg/kg) 15 a (expressed as caprolactam) Restrictions and specifications Korea (mg/l) 3 X YES NO 9-18 % (w/v) X YES NO 6 X NO YES ND b (expressed as isocyanate moiety) 1 mg/kg in final product expressed as isocyanate moiety 1-Hexadecanol NO YES X a : SML(T)[mg/kg] expressed as caprolactam b : 1 mg/kg in final product expressed as isocyanate moiety, 1 mg/kg in final product expressed as isocyanate moiety ND : The substance shall not migrate in detectable quantities X

39 OMVs from a Retort Pouch Film (PET/Al/PA/CPP) into the Different Fatty Food Simulants according to the Test Conditions in Different Countries USA Country FAP EU (Substitute test) Temp./time condition 121 /2 h 40 /10 d 37 Simulant 95% Ethanol Olive oil N- Heptane 7.1 d ± a ± FCN 40 /10 d 2.3 e ± d ± /3.5 h 0.9 e ± /6 h 0.8 e ± /2 h c ± /2 h b ± Korea & Japan 25 /1 h d ± 0.4 Abcde Means with the same superscrips are not significantly different (p>0.05). Each value is the mean of triplicate determinations.

40 57 Current Cell Developed Migration Cells Temp. resistance and leak proof against volatile solvents up to 150 were tested and assured. Improved Cells Single-sided migration 일반시약장 cell Korea Patent No Double-sided migration cell

41 Temperature Change in a SUS Migration Cell Filled with Olive Oil and Heated at 121 for 2 h :00:00 17:21:40 17:43:20 18:05:00 18:26:40 18:48:20

42 Migration into Dry Simulants Migration at higher temp. : liquid simulant and volatiles, oils unstable, degradation Simulant for dried foods Simulant for paper and PB Tenax, Porapak, Amberlite, active coal, and Celite were tested (Nerin et al., 2007; Lin et al., 2011). Main function as absorption of volatiles 39

43 Definition of Tenax Registered trademark for poly(2,6-diphenyl-p-phenyl oxide) (PPPO), modified polyphenylene oxide (MPPO), CAS No Porous polymer (500,000-1,000,000 Da) which efficiently traps volatiles. High surface area and low specific mass (0.23 g/cm 3 ) Official approval for migration testing as a dry food simulant (Simulant E) Recognized by the EC in the 2 nd amendment of Directive 82/711/EEC for testing plastics as a substitute test medium for fatty food. High thermal stability (ca. 350 ) Enables the use at high temperatures. 40

44 Limitation in the Use of Tenax Actual migration values can be different depending on experimental conditions such as particle size of Tenax, contact ratios, tightness of Petri dishes, and other extraction conditions (Barnkob and Petersen, 2013; Zurfluh et al., 2013; Han and Wang, 2014; Van den Houwe et al., 2016) Comparing tests : milk powder (Nerin et al., 2002), icing sugar (Aurela et al., 1999), flour and confectionary (Summerfiled and Cooper, 2001). For volatile substances, Tenax showed higher migration values comparing real foods, but lower values for non-volatile substances (Aurela et al., 1999). Tenax is evaluated to be superior for the use at high temperature for absorbing volatiles (Aurela et al., 2001) 41

45 Migration Tests Using Tenax (EU 10/2011) 42 Assigned for testing specific migration into dry foods. Overall migration 1) At high temperature (OM8, OM9) : Substitute test for OM7 2) Fresh (or chilled) fruits and vegetables 3) Dried fruits and vegetables (unpeeled and uncut) (RF=X/10)

46 43 Food Category Specific Assignment of Food Simulant (EU Reg. 10/2011)

47 Substituted Overall Migration Tests Using Tenax (EU 10/2011) 44 Test number OM 8 OM 9 Test conditions Food simulants E for 2 hours at 175 and food simulants D2 for 2 hours at 100 Food simulants E for 2 hours at 175 and food simulants D2 for 10 days at 40 Intended food contract conditions High temperature applications only High temperature applications including long term storage at room temperature Covers the intended food contract conditions described in OM1, OM3, OM4, OM5 and OM6 OM1, OM2, OM3, OM4, OM5 and OM6

48 Assignment of Tenax for Fruits and Vegetables Amendment of EU regulation 1416/2016 Reference number Description of food Food simulants Fruit, fresh or chilled : A. Unpeeled and uncut B. Peeled and/ or cut X X(*) Vegetable. Fresh or chilled : A. Unpeeled and uncut X/10 X/10 B. Peeled and/ or cut X X(*) 45

49 Food Products in Korea for Which Tenax is deemed to be Assigned As a Food Simulant (According to the EU Reg. 10/2011) 46 Product Manufacturer Product Picture Product Manufacturer Product Picture Bread Crown Convenience food Lotte Cookie St. Michel Vegetables Nonghyup Gums Lotte Tea Dongsuh Chocolate Andes Dried sardine Suhyup Fried dish Homeplus Margarine Ottogi

50 Food Products in Korea for Which Tenax is deemed to be Assigned As a Food Simulant (According to the EU Reg. 10/2011) 47 Product Manufacturer Product picture Product Manufacturer Product picture Vegetables Nonghyup Fruit Nonghyup Fruit Mariani Milk powder Ildongfoodis Starch Cheunwoo Sugar Beksul Sandwich Homeplus Bread E mart Cereal Post noodle Ottogi

51 An Example of the Necessity of Using a Dry Simulant Desiccant vials are designed to be used for dry foods and dietary supplements such as capsules and tablets for the long stability of products. Casings contain a significant amounts of various humectants (glycerin, fatty acid esters, mineral oils etc.) 48

52 OMVs from a Desiccant Vial depending on the Simulant Type 49 Food simulant Testing condition Dist. Water 70 / 30 min Extr. solvent Overall migration (mg/l) 1,550 Tenax Ether 68.8 Limitation (mg/l) 30

53 Validation of Efficiency for the Use of Tenax According to EU Testing Method (EN b) 50 Different migration behavior depending on the surrogates types Efficiency of ether for the extraction of Tenax Influence of the amounts of Tenax used Efficiency of migration testing condition 1) Spec. migration for dry foods : e.g. 40 /10 d, 100 /2 h 2) Overall migration (OM8, OM9) at high temp. : 175 /2 h Volatiles absorption : loss of volatiles at high temp. through the none-hermetically sealed Petri dish. Actual temperature condition Maintenance of absorption capacity of repeatedly used Tenax

54 Tested Film, Surrogates, and Experimental Conditions Tested film : LDPE/LLDPE copolymer, 45 μm Surrogates : 2,6-di-tert-butyl-p-cresol (BHT), tris (2,4-di-tert-butylphenyl) phosphate (Irgafos168), bis (2-ethylhexyl) adipate (DEHA), acetyl tributyl citrate (ATBC), diphenyl-1,2-phthalate (DPHP) Added conc. : 300 ppm each Migration condition of Tenax with film : 100 /1 h 51

55 52 Physical Properties of Surrogates Spiked to Tested Film Substance MG bp ( ) VP (mmhg at 25 ) Log p o/w CAS No. Use Diphenyl 1,2-phthalate (DPHP) E Bis(2-ethylhexyl) adipate (DEHA) Acetyl tributyl citrate (ATBC) Tris(2,4-di-t-butylphenyl) phosphite (Irgafos 168) E E Plasticizer Plasticizer Plasticizer E Antioxid. Butylated hydroxytoluene (BHT) E Antioxid.

56 53 OMVs depending on the Extraction Solvents Unit: mg/dm 2 Testing condition Extraction solvents Ether Ethanol Pentane Acetone 100 / 1 h 1.318±0.033 c 0.869±0.066 a 1.133±0.044 b 0.902±0.042 a Amounts of Tenax : 4 g/dm 2

57 54 OMVs depending on the Amounts of Tenax Unit: mg/dm 2 Extraction solvent Amount of Tenax (g/dm 2 ) Ether 0.754±0.035 a 1.324±0.040 b 1.365±0.035 b Heating temperature : 100 Heating time : 1 h

58 55 OMVs Depending on the Extraction Time and Temperature Unit: mg/dm 2 Extraction solvent Ether Amounts of Tenax : 4 g/dm 2 Testing condition 70 /1 h 100 /1 h 70 /2 h 100 /2 h 1.169±0.042 a 1.318±0.033 b 1.392±0.033 c 1.644±0.033 d

59 56 OMVs depending on the Leak Tightness of Petri dish Unit: mg/dm 2 Extraction solvent Ether Amounts of Tenax : 4 g/dm 2 Migr. Condition : 100 / 1 h * Petri dish was tightly wrapped with Al-foil Leak Tightness Open system Closed system* Without lid With lid 1.060±0.408 a 1.318±0.033 b 1.610±0.035 c

60 Conclusions 63 Korean regulations and testing methods for controlling FCMs need to be improved and globally harmonized. Some suggestions were made for the improvement of migration testing procedure, food simulants, and migration cells, etc. A pre-market control system for FCMs in Korea should be set-up with regard to the protection of consumers as soon as possible. Migration testing methods with Tenax need to be improved with more research works under different conditions. In the future, more efforts for the global harmonization of the migration testing methods and conditions, and the regulations are required.