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  • Development and application of a non-targeted extraction method for the analysis of migrating compounds from plastic baby bottles by GC-MS.

Development and application of a non-targeted extraction method for the analysis of migrating compounds from plastic baby bottles by GC-MS.

Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment (2014-11-20)
Matthias Onghena, Els van Hoeck, Philippe Vervliet, Marie Louise Scippo, Coraline Simon, Joris van Loco, Adrian Covaci
ABSTRACT

In 2011, the European Union prohibited the production of polycarbonate (PC) baby bottles due to the toxic effects of the PC monomer bisphenol-A. Therefore, baby bottles made of alternative materials, e.g. polypropylene (PP) or polyethersulphone (PES), are currently marketed. The principal aim of the study was the identification of major compounds migrating from baby bottles using a liquid-liquid extraction followed by GC/MS analysis. A 50% EtOH in water solution was selected as a simulant for milk. After sterilisation of the bottle, three migration experiments were performed during 2 h at 70°C. A non-targeted liquid-liquid extraction with ethyl acetate-n-hexane (1:1) was performed on the simulant samples. Identification of migrants from 24 baby bottles was done using commercially available WILEY and NIST mass spectra libraries. Differences in the migrating compounds and their intensities were observed between the different types of plastics, but also between the same polymer from a different producer. Differences in the migration patterns were perceived as well between the sterilisation and the migrations and within the different migrations. Silicone, Tritan™ and PP exhibited a wide variety of migrating compounds, whereas PES and polyamide (PA) showed a lower amount of migrants, though sometimes in relatively large concentrations (azacyclotridecan-2-one up to 250 µg kg⁻¹). Alkanes (especially in PP bottles), phthalates (dibutylphthalate in one PP bottle (±40 µg kg⁻¹) and one silicone bottle (±25 µg kg⁻¹); diisobutylphthalate in one PP (±10 µg kg⁻¹), silicone (up to ±80 µg kg⁻¹); and Tritan™ bottle (±30 µg kg⁻¹)), antioxidants (Irgafos 168, degradation products of Irganox 1010 and Irganox 1076), etc. were detected for PP, silicone and Tritan™ bottles. Although the concentrations were relatively low, some compounds not authorised by European Union Regulation No. 10/2011, such as 2,4-di-tert-butylphenol (10-100 µg kg⁻¹) or 2-butoxyethyl acetate (about 300 µg kg⁻¹) were detected. Migrating chemicals were identified as confirmed (using a standard) or as tentative (further confirmation required).

MATERIALS
Product Number
Brand
Product Description

Benzophenone, European Pharmacopoeia (EP) Reference Standard
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
Stearic acid, European Pharmacopoeia (EP) Reference Standard
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Anethol, natural, 99%, FG
Sigma-Aldrich
Ethyl alcohol, Pure, 190 proof, meets USP testing specifications
Sigma-Aldrich
Hexane, anhydrous, 95%
Sigma-Aldrich
Stearic acid, Grade I, ≥98.5% (capillary GC)
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Millipore
Ethyl acetate, suitable for HPLC, ≥99.8% (GC)
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
Sigma-Aldrich
4-Propylbenzaldehyde, 95%
Sigma-Aldrich
Ethyl acetate, anhydrous, 99.8%
Sigma-Aldrich
Ethyl alcohol, Pure, 190 proof, ACS spectrophotometric grade, 95.0%
Sigma-Aldrich
4-(Methylthio)benzaldehyde, 95%
Supelco
Benzophenone, analytical standard
Supelco
Melting point standard 79-81°C, analytical standard
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Supelco
Methyl laurate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Stearic Acid, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
4-tert-Octylphenol solution, 1000 μg/mL in acetone, analytical standard
Supelco
1,8-Cineole, primary reference standard
Supelco
Dichloromethane solution, contains 10 % (v/v) methanol
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Supelco
Stearic acid, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
Dichloromethane, suitable for HPLC, ≥99.8%, contains amylene as stabilizer
Sigma-Aldrich
Hexane, suitable for HPLC, ≥97.0% (GC)
Sigma-Aldrich
Ethyl acetate, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%