Evolving Food Packaging Regulations in Korea andupload.foodcontactscience.org/Uploads_Editor_File... · Evolving Food Packaging Regulations in Korea and ... Prohibit the use of DEHP

Keun Taik Lee

Dept. of Food Processing and Distribution

Gangneung-Wonju Nat. Univ., Rep. of Korea

Tel : +0082-33-640-2333, E-mail : [email protected]

Evolving Food Packaging Regulations in Korea and

Migration Testing with Tenax

2017 Food Contact Material Safety Symposium (Xian, China)

02. Nov. 2017

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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

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1

Restructuring History of Regulatory Bodies for FCMs

April 1996

Feb. 1998

June 2002

April 2009

: 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.

Mar. 2013

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MFDS NIFDS

Local authorities (Provinces, Counties, Cities etc.)

Legal actions

against violation

Response to the

inquiries from

public or industries

Safety evaluation

Risk assessment

Research

Inquiry Notice

Inquiry

Report

Governmental Safety Control System for FCMs

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Enacted by Act No. 1007

Jan. 1962

Apr. 1969 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)

Food Sanitation Act (FSA)

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Food Sanitation Act (FSA)

Chapter I General Provisions

I

Chapter III Apparatus, containers,

and packages

Chapter IV Labels

Chapter V Food Code

Chapter VI Inspection etc.

III

IV

V

VI

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

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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 ; 02.23.2015)

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)

Inspection of Domestic and Imported Food-Contact Utensils, Containers and Packages

Food Sanitation Act ; Article 19

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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.

Provisional Approval of the Standards and Specifications (FSA Ch. 3, Art. 9, Pg. 2 ② )

Food Sanitation Act (FSA)

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Standards and Specifications for Food

Utensils, Containers and Packages

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http://www.mfds.go.kr/eng/eng/index.do?nMenuCode=120&page=1&mode=view&boardSeq=70

089

English Website for the Standards and Specifications for FCMs in Korea

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I. General rules

II. Common standards and specifications

III. Specifications for individual materials

IV. Test methods

Standards and Specifications for Food Utensils, Containers and Packages

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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/m2

8) FCMs being used for plastics, cellophane, paper, starch shall not contain more

than 100 mg/kg (in total) Pb, Cd, Hg, and Cr+6.

11) Prohibit the use of DEHP in manufacturing FCAs, except where no migration

into foods is possible.

II. Common specifications and standards

Standards and Specifications for Food Utensils, Containers and Packages

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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

3. Specifications by material

Standards and Specifications for Food Utensils, Containers and Packages

II. Common specifications and standards

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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

Standards and Specifications for Food Utensils, Containers and Packages

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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, KMnO4 consumption etc.

4. Testing methods :

Standards and Specifications for Food Utensils, Containers and Packages

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Plastics

Acryl resin

Polyacetal (POM)

Ureaformaldehyde (UF)

Melamineformaldehyde (MF)

Phenolformaldehyde (PF)

Polyethyleneterephthalate (PET)

Polychlorovinylidene (PVDC)

Polystyrene (PS)

Polyethylene (PE), Polypropylene (PP)

Polyvinylchloride (PVC)

10

9

8

7

6

5

4

3

2

1

Polybutylene terephthalate (PBT)

Polymethacrylstyrene (MS)

Acrylonitrile-styrene (AS)

Acrylonitrile-butadiene-styrene (ABS)

Polybutene-1 (PB-1)

Polyurethane (PU)

Polyvinyl alcohol (PVA)

Polycarbonate (PC)

Polymethylpentene (PMP)

Nylon (PA) 11

12

13

14

15

16

17

18

19

- To be continued

Standards and Specifications for Food Utensils, Containers and Packages

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15

30

29

28

27

26

25

24

23

22

21

20 Epoxy resin

Polyethylene naphthalate(PEN)

Methylmethacrylate-acrylonitrile-butadiene-

styrene (MABS)

Ethylene vinyl acetate (EVA)

Ionomeric resin

Polyphenylene ether (PPE)

Fluoro resins (FR)

Polyacrylonitrile (PAN)

Hydroxybutyl polyester (HBP)

Polyarylate (PAR)

Polyarylsulfone (PASF)

36

35

34

33

32

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

Plastics

Standards and Specifications for Food Utensils, Containers and Packages

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(Heavy) Metals

Vinyl chloride

Vinylidene chloride

Styrene

Phenol

Formaldehyde

Melamine

Methylmethacrylate

Caprolactam

Bisphenol-A

Isocyanate

Acrylonitrile

Diphenyl carbonate

Tere- and isophthalic acid etc.

Lead

Cadmium

Mercury

Hexavalent chromium (Cr+6)

Antimony

Arsenic

Barium

Germanium

Chrome

Nickel

Barium

Zinc etc.

Monomers Additives etc.

DEHP

DEHA

PCBs

Fluorescence whitening agent

Toluene

BADGE, BFDGE

Dibutyl tin

Cresol phosphoric acid ester

Amines etc.

IV. Test methods

Standards and Specifications for Food Utensils, Containers and Packages

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Type of plastic

Details PVC PE/ PP PS PVDC PET PF MF UF POM

Acrylic

Resin

(1) Pb, Cd, Hg, Cr+6 1) 100 100 100 100 100 100 100 100 100 100

(2) Vinyl chloride 1 - - - - - - - - -

(3) Dibutyl tin compounds (as DBTD) 50 - - - - - - - - -

(4) Cresol phosphoric esters 1,000 - - - - - - - - -

(5) Volatile substances1)

(including styrene, toluene, ethylbenzene,

isopropyl benzene and n-propyl benzene)

- - 5,000 - - - - - - -

(6) Vinylidene chloride - - - 6 - - - - - -

(7) Barium - - - 100 - - - - - -

(8) BPA (including phenol, bisphenol A

and p-t-butyl phenol) - - - - - - - - - -

(9) Amines(triethyl amine and tributyl

amine)

(10) 1,3-Butadiene - - - - - - - - - -

1) As a sum

Standards and Specifications for Food Utensils, Containers and Packages

Residue specification (Plastics)

Unit : mg/kg

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Type of plastic

Details PVC PE/PP PS PVDC PET PF MF UF POM

Acryl

resin

(1) Pb 1 1 1 1 1 1 1 1 1 1

(2) KMnO4 consumption 10 10 10 10 10 - - - 10 10

(3) Overall Migration 301) 302) 303) 30 30 30 30 30 30 30

(4) Dibutyl phthalate 0.3 - - - - - - - - -

(5) Benzylbutyl phthalate 30 - - - - - - - - -

(6) Di-(2-ethylhexyl) phthalate 1.5 - - - - - - - - -

(7) Di-n-octyl phthalate 5 - - - - - - - - -

(8) Diisononyl phthalate 9 - - - - - - - - -

(9) Diisodecyl phthalate 9 - - - - - - - - -

(10) Di-(2-ethylhexyl) adipate 18 - - - - - - - - -

(11) 1-Hexene - 3(PE) - - - - - - - -

(12) 1-Octene - 15(PE) - - - - - - - -

(13) Ba - - - 1.0 - - - - - -

(14) Sb - - - - 0.04 - - - - -

(15) Ge - - - - 0.1 - - - - -

(16) Terephthalic acid - - - - 7.5 - - - - -

(17) Iso-phthalic acid - - - - 5 - - - - -

(18) Acetaldehyde - - - - 6 - - - - -

(19) Phenol - - - - - 5 5 5 - -

(20) Formaldehyde - - - - - 4 4 4 4 -

(21) Melamine - - - - - - 30 - - -

(22) Methylmethacrylate - - - - - - - - - 64)

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

Unit : mg/L

Standards and Specifications for Food Utensils, Containers and Packages

Migrant specification (Plastics)

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2006 • 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

• Fluorescent whitening agent from inner paper for chicken packages 2010

• Fluorescent whitening agent from pizza box 2010

Hot Issues on the Safety of Migrated Substances from FCMs

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2011 • 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

• PFCs from frying pan and paper tray 2015

• Bisphenol A from canned products 2015-2016

Hot Issues on the Safety of Migrated Substances from FCMs

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Safety Assurance Regulations for FCMs

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)

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PL for FCMs in Canada

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PL for FCMs in Japan

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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.

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.

Current Status and Challenges for the Reformation

of FCMs Regulations in Korea

Positive List System

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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.

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Opinions and Call for the Implementation of a PL System

for the FCMs in Korea

Required stricter control system for FCMs Increased necessity for implementing a positive

list system

The PL is stricter than the NL for

consumer protection

Status and suggestion for the safety control

system of FCMs

The Korea Food

Medical News

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http://news.jtbc.joins.com/article/article.aspx?news_id=NB11185544

JTBC News on 03. Mar. 2016

Insecure FCMs

No pre-market controls

for the FCMs in Korea Positive list systems in the

USA, EU and China

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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

(Baughan, 2006)

Factors that Influence Global Products Trade

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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

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Migration Testing Conditions and Specifications

Country Korea EU USA

Source Std. & Spec. for FCMs EU Reg. 10/2011

CEN, EN FAP FCN

For general use

(use at temperature ≤ 100℃)

Simple

(70℃/30 min or 25℃/1 h etc.) Very diverse and specified Diverse and specified

For the use at high temperature

(use at temperature ＞100℃)

Simple

(100℃/30 min) Very diverse and specified

Simple

(121℃/2 h or 66℃/2 h)

Simple

(121℃/2 h or

71℃/2 h)

Classification of

food types 4 types

6 types consisting of 83 different

food descriptions 10 types 4 types

Simulants/film area 2 ml/cm2 1 ml/cm2 (single side)

0.5 ml/cm2 (double side)

10 ml/ in2

(1.55 ml/cm2)

Extraction methods

Total immersion filling article,

single side contact using migration

cell

Total immersion (double), Tice cell

(single), standard pouch(single),

filling article (single) etc.

Total immersion, filling article,

single or double side contact using migration

cell etc.

Drying methods On hot plate after evaporation On hot plate after evaporation or

distillation On hot plate after evaporation

RF when using fatty food

simulant - 2-5 5 -

Limitation of OMVs Generally, ＜30 mg/l, except

when using n-heptane as a simulant

10 mg/dm2 film

60 mg/kg food or simulant

Different depending on

material type -

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Recommended Food Simulants

Recommended

simulants Aqueous Acidic Alcoholic Fatty Dry

EU 10% ethanol 3% acetic acid 20%3) or 50%4) ethanol Veg. oil MPPO

(Tenax)

USA

FAP1) Dist. water Dist. water or

3% acetic acid 8% or 50%5) ethanol n-Heptane None

FCN2) 10% ethanol 10% ethanol 10% or 50%6) ethanol Food oil, HB307,

Miglyol 812 None

Korea Dist. water 4% acetic acid 20% or 50%6) ethanol n-Heptane None

Japan

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

Veg. oil or

95% ethanol,

or n-Heptane

None

PVDC Dist. water 3% acetic acid 10% ethanol7) Olive oil or

95% ethanol None

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%.

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Migration Testing Conditions and Simulants for Different Food Types - I

Food type Country Test conditions for the foods stored or heated at

≤5℃ 20℃＜T≤40℃ 70℃ ≥100℃

Aqueous

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

USA

FAP 1) 21℃/2 d 49℃/1 d Fill boiling→ 38℃ 121℃/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

Japan

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

Acidic

EU Same as with aqueous simulant

USA

FAP 21℃/2 d 49℃/1 d Fill boiling→ 38℃ 121℃/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

Japan

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

1,2) Refer to the previous Table (Food simulants).

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Migration Testing Conditions and Simulants for Different Food Types - II

Food type Country Test conditions for the foods stored or heated at

≤5℃ 20℃＜T≤40℃ 70℃ ≥100℃

Alcoholic

EU Same as with aqueous simulant

USA 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 -

Japan

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

Fatty

EU Same as with aqueous simulant 100℃/2 h or at reflux or

121℃/1 h or 175℃/2 h

USA 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

Japan

MHLW 25℃/1 h 25℃/1 h 25℃/1 h 25℃/1 h

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).

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OMVs into Fatty Food Simulants (mg/dm2)

Polymer Thickness

(㎛)

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 30 2.1 1.4 3.4 2.0 1.5 1.4

LLDPE

30 3.3 1.4 7.6 2.9 2.3 2.3

60 1.3 1.0 3.7 2.1 1.3 1.2

80 4.4 2.8 6.4 3.2 1.7 0.9

CPP 50 1.9 1.3 3.5 2.4 1.6 1.0

80 4.6 4.4 7.6 4.3 1.6 1.3

OPP 20 3.1 2.6 7.1 4.2 1.1 1.7

40 2.2 1.2 3.3 2.6 1.3 1.1

PET 15 0.6 0.5 0.4 0.1 1.6 0.7

OPA 15 0.8 0.5 0.3 0.2 1.4 0.5

CPA 70 3.7 1.5 0.5 0.2 3.9 5.6

HIPS 1000 29.2 (79.2 mg/L) 16.1 57.1 24.3 3.7 4.0

GPPS-MPB 1000 50.6 (126.5 mg/L) 32.3 78.2 60.8 24.3 26.4

HIPS/EPS 200/2800 2.1 1.6 1.0 0.3 0.9 0.4

PVC 250 1.1 0.9 0.7 0.6 1.0 0.8

PP 3000 3.1 1.1 13.8 5.6 4.5 3.5

PVC wrap 13 41.0 (102.5 mg/L) 38.2 39.9 37.4 40.8 43.4

12 31.0 (77.5 mg/L) 26.8 32.0 30.7 34.4 32.0

LLDPE wrap 9 3.0 2.8 3.8 3.7 3.5 3.0

10 2.4 2.1 2.5 2.5 2.0 1.3

(Lee et al., 2002)

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Definition of Food Types according to the Migration Testing Methods

of EU, USA, and Japan or Korea

Food type

Type of Simulants

EU USA

Japan Korea FAP 1) FCN 2)

Aqueous pH>4.5 pH>5.0 - 3) pH>5.0 pH>5.0

Acidic pH≤4.5 pH≤5.0 - pH≤5.0 pH≤5.0

Alcoholic ＞6% Those containing

alcohol - ≥1% x

Fatty

Classified by the

description of

food type 4)

Those containing

fat - ≥20% x

1,2) Refer to the previous Table (Food simulants). 3) Categorized as defined in 21 CFR 176.170(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

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Substances Regulated in the EU or Korea (detected from a retort pouch composed of PET/Al/PA/CPP)

Substance

EU

Korea

(mg/L)

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

SML

(mg/kg)

Restrictions and

specifications

Caprolactam YES YES 15a

(expressed as caprolactam) 15

Butylated hydroxytoluene

(BHT)

YES

NO

3 X

Tris(2,4-di-tert-

butylphenyl )phosphate

(lrgafos 168)

YES NO 9-18 % (w/v) X

Octadecyl 3-(3,5-di-tert-

butyl-4-

hydroxyphenyl)propionate

(Irganox 1076)

YES NO 6 X

1-Isocyanato-3-

isocyanatomethyl-3,5,5-

trimethylcyclohexane

NO YES

NDb

(expressed as isocyanate

moiety)

1 mg/kg in final

product expressed as

isocyanate moiety

X

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

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OMVs from a Retort Pouch Film (PET/Al/PA/CPP) into the Different Fatty Food

Simulants according to the Test Conditions in Different Countries

37

Country Temp./time

condition

Simulant

95% Ethanol Olive oil N- Heptane

USA FAP

121℃ /2 h

→ 40℃ /10 d 7.1d ± 0.4 23.4a ± 4.4 -

FCN 40℃ /10 d 2.3e± 1.1 7.5d ± 2.4 -

EU

(Substitute test)

60℃ /3.5 h 0.9e ± 0.4 - -

60℃ /6 h 0.8e ± 0.3 - -

100℃ /2 h - 11.5c ± 0.1 -

121℃ /2 h - 19.5b ± 3.7 -

Korea & Japan 25℃ /1 h - - 1.3d ± 0.4

Abcde Means with the same superscrips are not significantly different (p>0.05).

Each value is the mean of triplicate determinations.

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57

Developed Migration Cells

일반시약장

Current Cell

Improved Cells ®

Temp. resistance and leak proof against volatile solvents

up to 150℃ were tested and assured.

Korea Patent No. 10-0491107

Double-sided migration cell

Single-sided migration cell

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119

94

70

46

22 ℃

17:00:00 17:21:40 17:43:20 18:05:00 18:26:40 18:48:20

Temperature Change in a SUS Migration Cell Filled with Olive

Oil and Heated at 121℃ for 2 h

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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

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Definition of Tenax®

Registered trademark for poly(2,6-diphenyl-p-phenyl oxide) (PPPO), modified

polyphenylene oxide (MPPO), CAS No. 24938-68-9.

Porous polymer (500,000-1,000,000 Da) which efficiently traps volatiles.

High surface area and low specific mass (0.23 g/cm3)

Official approval for migration testing as a dry food simulant (Simulant E)

Recognized by the EC in the ‘2nd 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.

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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)

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Migration Tests Using Tenax (EU 10/2011)

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)

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

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Substituted Overall Migration Tests Using Tenax (EU 10/2011)

44

Test number Test conditions Intended food contract

conditions

Covers the intended

food contract

conditions described in

OM 8

Food simulants E for 2

hours at 175 ℃ and food

simulants D2 for 2 hours

at 100 ℃

High temperature

applications only

OM1, OM3, OM4, OM5

and OM6

OM 9

Food simulants E for 2

hours at 175 ℃ and food

simulants D2 for 10 days

at 40 ℃

High temperature

applications including long

term storage at room

temperature

OM1, OM2, OM3, OM4,

OM5

and OM6

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Amendment of EU regulation 1416/2016

Assignment of Tenax for Fruits and Vegetables

45

Reference number Description of food Food simulants

‘04.01

Fruit, fresh or chilled :

A. Unpeeled and uncut

B. Peeled and/ or cut

X

X(*)

X/10

’04.04

Vegetable. Fresh or

chilled :

A. Unpeeled and uncut

B. Peeled and/ or cut

X

X(*)

X/10

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Food Products in Korea for Which Tenax is deemed to be

Assigned As a Food Simulant (According to the EU Reg. 10/2011)

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

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Food Products in Korea for Which Tenax is deemed to be

Assigned As a Food Simulant (According to the EU Reg. 10/2011)

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

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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.)

An Example of the Necessity of Using a Dry Simulant

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49

OMVs from a Desiccant Vial depending on the Simulant Type

Food simulant Testing condition Extr. solvent

Overall

migration

(mg/L)

Limitation

(mg/L)

Dist. Water

70℃/ 30 min

1,550

30

Tenax® Ether 68.8

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Validation of Efficiency for the Use of Tenax According to

EU Testing Method (EN 1186-13b)

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

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Tested Film, Surrogates, and Experimental Conditions

51

Tested film : LDPE/LLDPE copolymer, 45 ㎛

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

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Physical Properties of Surrogates Spiked to Tested Film

Substance

MG

bp

(℃)

VP

(mmHg at 25℃)

Log po/w

CAS No.

Use

Diphenyl 1,2-phthalate (DPHP) 318.33 403 7.92E-06 4.21 84-62-8

Plasticizer

Bis(2-ethylhexyl) adipate

(DEHA) 370.57 370.6 8.50E-07 8.12

103-23-1 Plasticizer

Acetyl tributyl citrate

(ATBC) 402.48 173 7.97E-07 4.29

77-90-7 Plasticizer

Tris(2,4-di-t-butylphenyl)

phosphite (Irgafos 168) 646.92 527 6.47E-09 13.6

31570-04-4 Antioxid.

Butylated hydroxytoluene

(BHT) 220.35 265 5.16E-03 5.10

128-37-0 Antioxid.

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OMVs depending on the Extraction Solvents

53

Testing condition

Extraction solvents

Ether Ethanol Pentane Acetone

100℃/ 1 h 1.318±0.033c 0.869±0.066a 1.133±0.044b 0.902±0.042a

Amounts of Tenax : 4 g/dm2

Unit: mg/dm2

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OMVs depending on the Amounts of Tenax

54

Extraction solvent

Amount of Tenax (g/dm2)

2 4 8

Ether 0.754±0.035a 1.324±0.040b 1.365±0.035b

Heating temperature : 100℃

Heating time : 1 h

Unit: mg/dm2

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OMVs Depending on the Extraction Time and Temperature

55

Extraction solvent Testing condition

70℃/1 h 100℃/1 h 70℃/2 h 100℃/2 h

Ether 1.169±0.042a 1.318±0.033b 1.392±0.033c 1.644±0.033d

Unit: mg/dm2

Amounts of Tenax : 4 g/dm2

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OMVs depending on the Leak Tightness of Petri dish

56

Extraction solvent

Leak Tightness

Open system Closed system*

Without lid With lid

Ether

1.060±0.408a 1.318±0.033b 1.610±0.035c

Amounts of Tenax : 4 g/dm2

Migr. Condition : 100℃/ 1 h

* Petri dish was tightly wrapped with Al-foil

Unit: mg/dm2

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Conclusions

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.

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