The sample was received in CETEA and was stored at approximately 23 C until being analysed.

Transcription

1 Test Report RE /09 INTERESTED PARTY: SGS Polímeros Ltda. Address: Estrada RS 122 Km 16 - Vila Progresso - São Sebastião do Caí /RS CEP ANALYZED MATERIAL: PVC film ANALISTS: Beatriz M. Curtio Soares, Caroline Donadon Torres, Joyce Borghetti and Sabrina Albino Lima DATE OF SAMPLE RECEPTION: August 19, 2009 Sample Description It was received for overall migration analysis in aqueous, acid and fatty simulant a sample of PVC film. According to the client, the PVC film was manufactured by BandFilmes with the Olvex 51 plasticizer additive which is manufactured by SGS Polímeros. The film was confectioned with Braskem sp1300 resin and was 10 μm thick. The sample was received in CETEA and was stored at approximately 23 C until being analysed. Method The evaluations of overall migration was accomplished according to the procedures and rules established in Resolution 105 of May 19, 1999, published by the Brazilian Sanitary Surveillance Agency (Agência Nacional de Vigilância Sanitária) of the Brazilian Ministry of Health in Diário Oficial da União (Federal official gazette in which all Brazilian Federal Laws and Regulations are published) of May 20, This Resolution contains the Brazilian and MERCOSUL harmonized laws and regulations that apply to plastic packages and equipments intended to come into contact with foodstuffs. According to the interested party, the PVC film is intended to come into contact with foods and beverages in general non-alcoholic, at temperatures up to 40 C, therefore, the sample was evaluated in the contact conditions presented in Table 1, considering the following food classification and respective simulants: TYPE I: non-acid aqueous foods (ph>5) for which distilled water is used as simulant; TYPE II: acid aqueous foods (ph 5) for which a solution of acetic acid in distilled water at 3% (w/v) is used as simulant; TYPE III: a. aqueous, non-acid foods containing oil or fat, for which distilled water and n-heptane or olive oil are used as simulants; b. aqueous, acid foods containing oil or fat, for which a solution of acetic acid in distilled water at 3% (w/v) and n-heptane or olive oil are used as simulants; TYPE IV: oily or fatty foods, for which n-heptane or olive oil are used as simulant; TYPE VI: solid, dry foods or foods with no or little extraction power. For this group of foodstuffs, no migration tests are required. Occasionally, tests to verify compliance of packaging materials with overall migration limits may be required. In such cases, migration tests are performed using distilled water, a solution of acetic acid 3% in distilled water, a solution of ethanol 10% or 15% in distilled water or n-heptane or olive oil as simulant, depending on the type of foodstuff. Tradução 1/5 CENTRO DE PESQUISA E DESENVOLVIMENTO DE EMBALAGENS (CENTRO DE TECNOLOGIA DE EMBALAGEM) Av. Brasil, 2880 CEP Campinas/SP Brasil Tel Fax

2 TABLE 1. Conditions of time and temperature used in the overall migration tests. Simulants Distilled water Solution of acetic acid in distilled water at 3% (w/v) Olive Oil Contact condition The methodology to quantify the overall migration in aqueous simulants consisted of the sample contact with extraction solutions in certain periods and temperatures that simulated their actual condition of use. The residues of overall migration were determined by the weight difference after the contact and evaporation of the solutions using an analytical scale with 0.01 mg of accuracy. The PVC film was evaluated as for migration using olive oil as fatty simulant according to the methodology Determination of overall migration of plastic materials using olive oil as a fatty simulant, described in Annex VI of Resolution published by ANVISA, considering a long term contact at room temperature, that is, an essay condition at 40 ºC ± 5 ºC for 10 days. In this analysis a specimen with known area and weight was immersed and remained in contact with the olive oil in selected conditions of time and temperature. At the end of the contact period, the test specimen was dried between sheets of filter paper Whatman nº1 and weighed. The oil absorbed by the test specimen was, then, extracted in Soxhlet with hexane during 18 hours and its weight was determined by gas chromatography after saponification and methylation of the fatty acids. The mass of the oil absorbed was used as a correction factor for the calculation of overall migration. Before and after the contact with olive oil, the specimens were conditioned at 23 ºC ± 2 ºC and 50%RH ±5%RH until constant weight. The chromatographic analysis was carried out in a HP5890 gas chromatograph with flame ionization detector, operating with a fused silica capillary column HP1 (polydimethylsiloxane) with 50 m and internal diameter of 0.22 mm. The quantification of the mass of oil absorbed was made by gas chromatography, using the peak of methyl ester of oleic acid C 18:1 (methyl oleate) as reference and external standardization. The overall migration was expressed in mg/dm². Results The results of the overall migration tests on the PVC film are shown in Table 2. TABLE 2. Residues of overall migration obtained for the PVC film in mg/dm 2(1). Simulants Contact Condition Mean Standard Deviation Interval of Variation Distilled water (2) 7.6 Solution of acetic acid in distilled water at 3% (w/v) (2) 6.7 Olive Oil (1) Result of four determinations (2) Correspond to the quantification limit of the method, under the analytical conditions Tradução 2/5

3 Those results take into account what is currently in force according the Resolution published by ANVISA regarding the requirements of overall migration using olive oil as a fatty simulant, the sample treatment and interpretation of results, with the exception of the analytical tolerance that is specified in Directive 2002/72/EC. After the publication of Draft Resolution 30 of May 26, 2009, these values will change, because other rules will be adopted for treatment of the sample. All the analyzed specimens of the PVC film, after the contact with the fatty simulant olive oil, presented perceptible visual modification, losing the original flexibility. The maximum limit of overall migration established in Resolution is of 8.0 mg of residue per dm 2 of plastic material, with an analytical tolerance of 10% in the analysis with the aqueous simulants. Therefore 8.8 mg/dm 2 is the maximum tolerable value. The overall migration results obtained in the analysis with the simulants distilled water and acetic acid solution, under the applied contact conditions, were below the established limits. The analytical tolerance for the analysis with olive oil as simulant is 3.0 mg/dm 2. This analytical tolerance indicates that the mean of the results of the four determinations could vary between 9.5 mg/dm 2 and 15.5 mg/dm 2. The Resolution permits the use of reduction factors in order to adapt the extractive power of the olive oil to the actual extractive potential of some food categories, which are applied dividing the result of the overall migration by values varying from 2 to 5, depending on the food. According to Resolution , the food categories that permit the use of 2 as reduction factor are: Margarine, butter and other fats and oils made from water emulsions in oil; According to Resolution , the food categories that permit the use of 3 as reduction factor are: Confectionery products in paste form: with fatty substances on the surface; Nuts (peanuts, chestnuts, almonds, hazelnuts, walnuts, pine kernels and other) in paste or cream form; Fish fresh, chilled, salted, smoked or in the form of paste; All others cheeses that are not whole with rind or processed cheeses; Preparations for soups, broths (extracts, concentrates), homogenized composite food preparations, prepared dishes liquid or paste: with fatty substances on the surface; Mayonnaise, sauces derived from mayonnaise, salad creams and other oil in water emulsions; Mustard (except powdered mustard); Cocoa paste. According to Resolution , the food categories that permit the use of 4 as reduction factor are: Meat of all zoological species (including poultry and game): fresh, chilled, salted, smoked or in the form of paste, creams; Processed meat products (ham, salami, bacon and other); Fried or roasted foods: of animal origin. Tradução 3/5

4 According to Resolution , the food categories that permit the use of 5 as reduction factor are: Pastry, biscuits, cakes and other bakers wares, dry: with fatty substances on the surface; Pastry, cakes and other bakers wares, fresh: with fatty substances on the surface; Chocolate, sugar and products thereof Confectionery products: chocolate, chocolate-coated products, substitutes and products coated with substitutes; Confectionery products in solid form: with fatty substances on the surface; Nuts (peanuts, chestnuts, almonds, hazelnuts, walnuts, pine kernels and other: Shelled and roasted; Fried or roasted foods: fried potatoes, fritters and the like; Preparations for soups, broths, in liquid, solid or powder form (extracts, concentrates), homogenized composite food preparations, prepared dishes: with fatty substances on the surface; Sandwiches, toasted bread and the like containing any kind of foodstuff: with fatty substances on the surface; Dried foods: with fatty substances on the surface; Cocoa powder. Conclusions As far as the overall migration to distilled water and solution of acetic acid in distilled water at 3% (w/v), the sample of PVC film with 10 μm thick manufactured by BandFilmes with Braskem sp1300 resin and Olvex 51 plasticizer additive meet the specification laid down in Resolution considering a long term contact at temperatures up to 40 C with foods and beverages Types I, II and VI; As far as the overall migration to olive oil, the sample of PVC film with 10 μm thick manufactured by BandFilmes with Braskem sp1300 resin and Olvex 51 plasticizer additive meet the specification laid down in Resolution considering a long term contact at temperatures up to 40 C with oily or fatty foods and beverages listed above (Types IIIa and b in relation to fat content and Type IV), with categories for those Resolution defines 2, 3, 4 or 5 as reduction factor. When the Draft Resolution 30 of May 26, 2009 is published, these conclusions will change, because other rules will be adopted for treatment of the sample. This document does not exclude the necessity to prove that the composition of the film are all food contact substances (positive lists) nor the need of complementary tests that may be necessary, for full compliance with the food contact approval law. The assay presented in this report is part of the target of the qualification of CETEA/ITAL by the Rede Brasileira de Laboratórios Analíticos em Saúde - REBLAS (Brazilian Net of Analytical Laboratories on Health). However, the interpretations of the results are not part of this target. References BRASIL. Agência Nacional de Vigilância Sanitária. Resolução nº 105, de 19 de maio de Aprova os Regulamentos Técnicos: Disposições Gerais para Embalagens e Equipamentos Plásticos em contato com Alimentos e seus Anexos. Diário Oficial da República Federativa do Brasil, Brasília, DF, May, 20 th, Section 1, p Available in: Access in: December, 09, Tradução 4/5

5 THE COMMISSION OF THE EUROPEAN COMMUNITIES. Corrigendum to Commission Directive 2002/72/EC, of 06 August Relating to plastic materials and articles intended to come into contact with foodstuffs. Official Journal of the European Union, L 220, Luxembourg, p. L 39/42, 13 feb Available in: < >. Access in: dec., 14, Observations This work was accomplished with calibrated equipments and inspection, measuring and testing instruments. Their total uncertainties are in agreement with the acceptance criteria established by the Quality Management System of ITAL and were not considered in the calculation of the presented results, but can be made available to the interested party, under formal request. This Report is in agreement with CETEA Internal Norm CE 017 Elaboration and Sending of Reports. The test results contained in this report apply solely to the sample sent to CETEA for evaluation. This Report may be published only in its entirely. Partial reproduction of this Report requires written consent of this Center. Documents and registers of this job, as well as the copy of this report, will be kept by CETEA for a period of 5 years. This report is only valid with the original signatures or rubric in all pages. English version of the Test Report RE /09. In case there is any doubt, the Portuguese version of the Test Report RE /09 prevails. Campinas, March 10 th, Joyce Borghetti Analytical Technological Researcher Eloisa Elena Corrêa Garcia Manager - Plastic Packages and Environment RAm 1018/09 GSN Tradução 5/5