[Application of High-performance Liquid Chromatography to Caprolactam Migration Testing of Food Utensils, Containers, and Packaging].

We assessed the applicability of high-performance liquid chromatography (HPLC) to the official testing method for the migration of caprolactam (CPL) from food utensils, containers, and packaging made from polyamide (PA). Hydrophilic interaction chromatography (HILIC) columns coated with unmodified silica, carbamoyl, and aminopropyl were used. Water and acetonitrile (ACN) were used as the mobile phase, and the analytical conditions were optimized.

[Plasticizers Used in Polyvinyl Chloride Toys (2019-2020)].

We determined the fifteen types of plasticizers, including four kinds of phthalic acid esters (PAEs) used in 220 polyvinyl chloride (PVC) toys on Japanese market from 2019 to 2020. Three kinds of previously undetected types of PAEs were also detected, but not identified in this study. Di (2-ethylhexyl) terephthalate (DEHTP) was the highest detection rate in 209 soft PVC toys out of 220 toys, with 71.

[Modified Methods for Analyzing Bisphenol A Content for Migration Tests from Polycarbonate Food Apparatuses, Containers, and Packaging].

A validation study was performed on the modified analytical method for the migration solution of heptane, 20% ethanol and 4% acetic acid for the determination of bisphenol A migrating from polycarbonate food apparatuses, containers, and packaging. The analytes for the method were bisphenol A, phenol and p-tert-butylphenol. The repeatability, within-laboratory reproducibility and trueness of the method was estimated in the range of 0.

[Study on Migrants Found in Migration Solutions from Commercially Available Polyethylene Products].

Migrants found in migration solutions obtained from commercially available polyethylene products that may contain food were studied and analysed via liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF) for non-target screening and LC-MS/MS for quantifying 14 substances in migration solutions. Furthermore, an analytical approach based on the retention gap was developed for accurate separation techniques using LC-MS/MS. Irganox 1076 was detected at a maximum of 1.

Determination of potential volatile compounds in polyethylene terephthalate (PET) bottles and their short- and long-term migration into food simulants and soft drink.

Head space (HS)-GC-MS was used to analyze possible migration of volatile compounds from polyethylene terephthalate (PET) bottles for soft drinks, and a total of six compounds were identified. Next, a rapid, simple, and accurate simultaneous method was established using purge-and-trap (PT)-GC-MS, to quantify their amounts in the liquid contents after short- and long-term storage in PET bottles. Starting with brand-new PET bottles, the maximum migration of 2-methyl-1,3-dioxolane into distilled water and 50 % aqueous ethanol after 2 years at 25 °C were 2.

[Inter-laboratory Study on the Modified Method Assessment for the Determining Methanol Content in Kitchen Detergents].

We modified a method for determining methanol content in detergents used in kitchens. Furthermore, an inter-laboratory study was conducted in 10 laboratories to validate the modified method. In this study, two concentrations of samples were blindly coded.

[Validation Study on Migration Test for Plastic Food Utensils, Containers, and Packaging].

Migration test of food utensils, containers, and packaging is an important test method for confirming the safety and their compliance to the standards. However, there is little report on inter-laboratory study which was performed to evaluate the entire migration test, including migration operations and quantification. An interlaboratory study was performed participating 22 laboratories using 8 types of model synthetic resin samples containing 10 substances with a wide range of Log P values to evaluate the accuracy of the entire migration test.

Determination of formaldehyde and acetaldehyde levels in poly(ethylene terephthalate) (PET) bottled mineral water using a simple and rapid analytical method.

A simple and rapid analytical method was developed for the determination of formaldehyde (FA) and acetaldehyde (AA) contents in water. FA and AA were derivatized by 2,4-dinitrophenylhydrazine in an LC vial for 20 min at room temperature, about 25 °C, and analyzed using LC-MS/MS. The calibration curve exhibited excellent linearity for FA and AA concentrations of 2-150 ng/mL.

Rapid identification of polyamides using direct analysis in real time mass spectrometry.

Rationale: Polyamide (PA) is the generic name of polymers synthesized by linking monomers via amide bonds, and various types of PAs with different monomer compositions are known. Distinguishing PA polymers is useful in directing monomer residual testing, product testing, and reverse engineering, but is analytically challenging and cumbersome. To simplify this, we explored the applicability of direct analysis in real time mass spectrometry (DART-MS) for screening PA polymers.

[Consideration of the Evaporation Residue Test for Plastics Intended to Contact with Oils and Fatty Foods].

The Japanese Food Sanitation Act designates the evaporation residue test as a specification for plastics that intended to contact with foods. The test conditions and migration limits for oils and fatty foods were considered on the basis of the results obtained from the evaporation residue test according to the Japanese Act and the overall migration test into olive oil according to EN1186-2. The evaporation residue test was conducted using heptane at 25℃ for 1 hour.

[Headspace GC/MS Analysis of Residual Solvents in Laminated Films Used for Food Packaging].

Multilayer laminated films may contain organic solvents derived from adhesives, printing inks and so on. A headspace-GC/MS analysis method for the simultaneous determination of 30 substances such as toluene, xylene, acetone, methyl ethyl ketone, ethyl acetate, butyl acetate, methanol, ethanol, was developed. A N,N-dimethyl formamide solution containing an internal standard substance was added to the sample.

[Changes in Status of Plasticizers Used in Polyvinyl Chloride Toys].

Analytical survey of plasticizers used in about 500 polyvinyl chloride (PVC) toys in Japanese market was performed in 2014. The results obtained were compared with those obtained in 2009. Fifteen types of plasticizers including di (2-ethylhexyl) terephthalate (DEHTP) were detected.

[Establishment of Test Methods for Overall Migration Test into Vegetable Oil Applied to Food Contact Materials Intended for Contact with Oils and Fatty Foods].

The evaporation residue test designated in the Japanese Food Sanitation Act is used to determine the total migration amount of substances that food contact materials release into foods. Vegetable oil would be the most suitable food simulant for oils and fatty foods, but it is difficult to remove by heating due to its high boiling point, so heptane and 20％ ethanol are used as substitute food simulants in the test for plastics and rubbers. The EU has introduced an overall migration test into olive oil for plastics intended to come into contact with oils and fatty foods.

[Interlaboratory Study on Evaporation Residue Test for Food Contact Products (Report 2)].

An interlaboratory study was performed to evaluate the equivalence between an official method and a modified method of evaporation residue test using heptane as a food-simulating solvent for oily or fatty foods, based on the Japanese Food Sanitation Law for food contact products. Twenty-three laboratories participated, and tested the evaporation residues of nine test solutions as blind duplicates. In the official method, heating for evaporation was done with a water bath.

[Interlaboratory Study on Evaporation Residue Test for Food Contact Products (Report 1)].

An interlaboratory study was performed to evaluate the equivalence between an official method and a modified method of evaporation residue test using three food-simulating solvents (water, 4% acetic acid and 20% ethanol), based on the Japanese Food Sanitation Law for food contact products. Twenty-three laboratories participated, and tested the evaporation residues of nine test solutions as blind duplicates. For evaporation, a water bath was used in the official method, and a hot plate in the modified method.

Migration of nonylphenol and plasticizers from polyvinyl chloride stretch film into food simulants, rapeseed oil, and foods.

Nonylphenol (NP) has been suspected as an endocrine-disrupting chemical. Japanese polyvinyl chloride (PVC) stretch films contained 0.5-3.

[Interlaboratory Study on Caprolactam Test for Food-Contact Nylon Products].

The Japanese Food Sanitation Law sets a limit on the migration level of caprolactam for food-contacting nylon products. Here, we carried out an interlaboratory study in twenty laboratories to evaluate the performance of the official GC-FID test method and a GC-MS method as an alternative test method to the official method. Each laboratory quantified caprolactam in three test solutions in 20% ethanol as blind duplicates using GC-FID or GC-MS.

[Interlaboratory Study on Volatiles Test for Food-Contacting Polystyrene Products].

Using polystyrene, acrylonitrile-styrene resin and acrylonitrile-butadiene-styrene resin pellets as samples, an interlaboratory study was performed to evaluate the volatiles test method, based on the specifications described in the Japanese Food Sanitation Law for food-contacting polystyrene products. The study was conducted with the participation of twenty-one laboratories. Each laboratory quantified the contents of styrene, toluene, ethylbenzene, isopropylbenzene and propylbenzene in three test pellets using GC-FID, GC-MS or headspace-GC-FID.

Isolation and Quantification of Polyamide Cyclic Oligomers in Kitchen Utensils and Their Migration into Various Food Simulants.

Small amounts of cyclic monomers and oligomers are present in polyamide (PA)-based kitchen utensils. In this study, we isolated eight PA-based cyclic monomers and oligomers from kitchen utensils made from PA6 (a polymer of ε-caprolactam) and PA66 (a polymer of 1,6-diaminohexane and adipic acid). Their structures were identified using high-resolution mass spectrometry and 1H- and 13C-nuclear magnetic resonance spectroscopy, and their residual levels in PA-based kitchen utensils and degree of migration into food simulants were quantified by high-performance liquid chromatography/mass spectrometry using purchased PA6 monomer and isolated PA66 monomers, and isolated PA6 and PA66 oligomers as calibration standards.

[Survey of Primary Aromatic Amines and Colorants in Polyurethane, Nylon and Textile Toys].

The residual and migration levels of 28 primary aromatic amines (PAAs) in polyurethane and nylon toys were determined using LC-MS/MS, and the migration and residual amounts of PAAs and 15 colorants in textile toys were determined using LC-MS/MS and LC-TOF-MS according to the European Standard EN71. Among 34 polyurethane toy samples, 2,6-diaminotoluene and 2,4-diaminotoluene were detected in the same 12 samples at residual levels ranging from 2.1 to 19.

[Interlaboratory Study on Zinc Test for Food-Contact Rubber Products].

Using six kinds of zinc solution in water and 4% acetic acid as samples, an interlaboratory study was performed to evaluate a zinc (Zn) test method for food-contact rubber products, based on the Japanese Food Sanitation Law. Eighteen laboratories participated, and quantified Zn in six test solutions as blind duplicates using flame atomic absorption spectrometry, induced coupled plasma-optical emission spectrometry or induced coupled plasma-mass spectrometry. Statistical analysis revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 97-103%, 0.

[Interlaboratory study on migration test of antimony and germanium for food-contact polyethylene terephthalate].

An interlaboratory study was performed to evaluate a migration test method of antimony (Sb) and germanium (Ge), based on the Japanese Food Sanitation Law for food- contact polyethylene terephthalate. Eighteen laboratories participated, and quantified Sb and Ge in three test solutions as blind duplicates using graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma-optical emission spectrometry (ICP-OES) or induced coupled plasma-mass spectrometry (ICP-MS). Statistical analysis revealed that the trueness, repeatability and reproducibility were 98-107%, 1.

Identification and Quantitation of Volatile Organic Compounds in Poly(methyl methacrylate) Kitchen Utensils by Headspace Gas Chromatography/Mass Spectrometry.

A headspace GC/MS method was developed for identification and quantitation of residual volatile organic compounds in poly(methyl methacrylate) (PMMA) kitchen utensils. A sample was cut into small pieces, then N,N-dimethylacetamide was added in a headspace vial and sealed. After storing for more than 1 day at room temperature, the vial was incubated for 1 h at 90°C, and the headspace gas was analyzed by GC/MS.

[Interlaboratory study on migration test of cadmium and lead for food contact articles].

An interlaboratory study was performed to evaluate a migration test method of cadmium (Cd) and lead (Pb), based on the Japanese Food Sanitation Law for glassware, ceramicware, enamelware and metal cans. Seventeen laboratories participated, and quantified Cd and Pb in eight test solutions as blind duplicates using flame atomic absorption spectrometry (AAS), graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma-optical emission spectrometry (ICP-OES) or induced coupled plasma-mass spectrometry (ICP-MS). Statistical analysis revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 93-105%, 0.

Survey of volatile substances in kitchen utensils made from acrylonitrile-butadiene-styrene and acrylonitrile-styrene resin in Japan.

Residual levels of 14 volatile substances, including 1,3-butadiene, acrylonitrile, benzene, ethylbenzene, and styrene, in 30 kitchen utensils made from acrylonitrile-butadiene-styrene resin (ABS) and acrylonitrile-styrene resin (AS) such as slicers, picks, cups, and lunch boxes in Japan were simultaneously determined using headspace gas chromatography/mass spectroscopy (HS-GC/MS). The maximum residual levels in the ABS and AS samples were found to be 2000 and 2800 μg/g of styrene, respectively. The residual levels of 1,3-butadiene ranged from 0.