Large volume headspace GC/MS analysis for the identification of volatile compounds relating to seafood decomposition.

Decomposition in seafood products in the United States is monitored by the Food and Drug Administration (FDA) laboratories using sensory testing, which requires highly trained analysts. A large-volume headspace (LVHS) gas chromatography/mass spectrometry (GC/MS) method was developed to generate analytical results that can be directly compared to sensory evaluation. Headspace vapor was withdrawn from a 1-L vial containing 50 g seafood sample using a large volume headspace autosampler. Various volatile compounds were collected simultaneously. Analytes were preconcentrated by a capillary column trapping system and then sent through a cryo-focuser mounted onto the GC injector. A selected ion monitoring (SIM) MS acquisition method was used to selectively monitor 38 compounds of interest. Samples of red snapper, croaker, weakfish, mahi-mahi, black tiger shrimp, yellowfin tuna, and sockeye salmon that have been assessed and scored by an FDA National Seafood Sensory Expert (NSSE) were used for method performance evaluation. Characteristic compounds potentially associated with seafood quality deterioration for each seafood species were identified by quantitative analysis using pooled matrix-matched calibrations and two-sample t-test statistical analysis. Classification of fresh and decomposed samples was visualized on the analysis of variance (ANOVA)-principal component analysis (PCA) score plots. The results determined that the LVHS-GC/MS technique appeared promising as a screening tool to identify compounds representative of sensory analysis.

Extraction and analysis of an organophosphate salt nucleating agent from irradiated polypropylene resin.

Although it is well-established that irradiation of produce can reduce food-borne pathogens and spoilage organisms, data on the effect of irradiation on polymer additives in food packaging materials are limited, particularly for those additives used in packaging leafy greens or in current food packaging materials. We investigated the effects of irradiating a nucleating agent, aluminium, hydroxybis[2,4,8,10-tetrakis(1,1-dimethylethyl)-6-hydroxy-12H-dibenzo [d,g][1,3,2]dioxaphosphocin 6-oxidato]- (CAS Reg. No. 151841-65-5), at doses of 1-20 kGy in polypropylene. That nucleating agent was then extracted using accelerated solvent extraction and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), liquid chromatography-photodiode array detection (LC-PDA), and solid-state nuclear magnetic resonance (SSNMR) spectroscopy. We found this nucleating agent was not significantly affected by radiation treatment up to 20 kGy. Therefore, this nucleating agent could potentially be useful in food packaging materials that will be irradiated at doses of 20 kGy or less. Establishing which additives are stable under anticipated irradiation doses will help support safety evaluation of food packaging materials.

Evaluation of portable vibrational spectroscopy for identifying plasticizers in dairy tubing.

Plasticisers are commonly used to increase the flexibility of a wide variety of food contact materials including the plastic tubing, liners, and gaskets used in the dairy industry. In recent years, some classes of plasticisers have come under scrutiny due to the potential for transfer of these compounds into the milk itself, which can then be further processed into foods such as powdered milks and cheeses, infant formula, and baked goods. One such set of plasticisers that is being evaluated for frequency of use, potential routes of exposure, and risk to consumers is ortho-phthalates, hereafter referred to as phthalates. In order to better understand the actual use of phthalate versus non-phthalate plasticised tubing, a robust, rapid, and portable analytical method is necessary for on-site screening. Laboratory Raman and near-infrared spectrometers have been used extensively for polymer and additive evaluation, and advances in portable/hand-held technology could lead to feasible plasticiser evaluation in the field. This research overviews efforts to evaluate six portable spectroscopy devices for their ability to identify phthalate versus non-phthalate plasticised polyvinyl chloride (PVC) dairy tubing, liners, and gaskets. The most successful method, a hand-held Raman spectrometer along with a plasticiser spectral library or a chemometric model, can rapidly and accurately identify phthalate containing PVC and has the potential to be employed as a future field screening technique for regulators and the dairy industry.

Analysis of per- and poly-fluoroalkyl substances (PFAS) in processed foods from FDA's Total Diet Study.

Additional occurrence data are needed to better understand human exposure to per- and poly-fluoroalkyl substances (PFAS) from commercially available foods in the United States. The Food and Drug Administration's (FDA) Total Diet Study (TDS) collects foods that are both nationally and regionally distributed. In 2018, 172 processed foods were collected from grocery stores around Lenexa, KS, as part of the TDS national collection. A previously developed method for the analysis of PFAS in foods as part of the TDS regional collection was modified and optimized for these samples. This method was single lab validated using 5 different matrices and method detection limits were calculated. During the analysis of these samples, challenges arose with method blanks and further investigation into statistical methods to distinguish between blank and sample concentrations were done. The confirmation of two short chain PFAS, perfluorobutanoic acid (PFBA) and perfluoropentanoic acid (PFPeA), was not possible using triple quadrupole mass spectrometry and a confirmation method was developed using high-resolution mass spectrometry. This technique was also used to investigate potential detections and interferents that fell within the retention time criteria for positive detections. In the national collection, positive detections of perfluorooctanesulfonic acid (PFOS) and perfluorononanoic acid (PFNA) were found in frozen fish sticks/patties, PFOS and perfluorodecanoic acid (PFDA) in canned tuna, and PFOS in protein powder. Concentrations were all below 150 ppt, and no other detects were confirmed above the method detection limits in any other foods.

Method Development and Validation of Per- and Polyfluoroalkyl Substances in Foods from FDA's Total Diet Study Program.

Human exposure to per- and polyfluoroalkyl substances (PFAS) through the US diet has not been well-characterized. Highly consumed foods are routinely monitored through FDA's Total Diet Study program. Portions of these samples were used to develop and validate a method for PFAS in a wide variety of foods. The extraction of 16 PFAS was performed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and analyzed by liquid chromatography/mass spectrometry. Method optimizations are described including investigations into the QuEChERS sorbents, matrix effects, and solid-phase extraction (SPE) cartridges. The use of a custom push-through SPE cartridge showed promising results as a rapid cleanup option for food samples. Challenges in ion confirmation are discussed, and the use of enhanced product ion (EPI) full-scan MS/MS spectra is presented as a potential option for verifying false positives. The validated method was then used for the analysis of 179 total diet study samples, and positive detects for perfluorooctanesulfonic acid (PFOS) were found in two fish and one meat sample.

Determination of phthalate concentrations in paper-based fast food packaging available on the U.S. market.

Phthalates are one of many chemical compounds that are used as plasticisers. Packaging can transfer plasticisers to the surfaces of foods or other materials. A recent study suggested a link between fast food consumption and increased urine phthalate metabolites even though phthalates are most commonly found in food contact materials made of PVC while fast food packaging is most commonly composed of paper and paper board. Phthalates in PVC are usually present in percent concentrations. In non-PVC food contact materials, such as paper or paperboard, the concentrations, if any, are expected to be significantly lower which can greatly impact the analytical method used for their determination. Due to the widespread use of plasticised PVC in many commercial applications, background concentrations of phthalates are a concern for trace concentration analyses and background contamination must be avoided when performing these analyses. A glassware cleaning method was developed and a solvent extraction with dichloromethane and hexane was used to extract phthalates from paper-based food packaging. The extracts were then analysed using a GC-MS/MS. The minimum reporting concentrations for the method were determined to be 0.10-0.40 µg/g depending on the phthalate investigated. Phthalate concentrations in several different non-PVC printed and unprinted packaging are presented. Of the 54 packaging samples tested, 10 samples contained no reportable concentrations of any of the 6 phthalates investigated. Of those that were reportable, all measured lower than 10 µg/g and in fact, most had concentrations less than 1 µg/g. These data demonstrate that phthalates from fast food packaging do not significantly contribute to overall consumer exposure.

Migration of phenolic brominated flame retardants from contaminated food contact articles into food simulants and foods.

Several food contact articles (FCAs) contaminated with unapproved brominated flame retardants (BFRs) purchased in the US market were analysed and subjected to migration tests. Migration tests were performed in food simulants (water, 3% acetic acid, 10% ethanol and 50% ethanol) and food (milk, coffee and chicken bouillon soup) to evaluate the BFRs mass transfer from the contaminated FCA. The BFRs studied, 2,4,6-tribromophenol (TBP), 3,3',5,5'-tetrabromobisphenol A (TBBPA), and 1,2,5,6,9,10-hexabromocyclododecane (HBCD) were analysed by UHPLC-MS/MS. The method validation parameters were r2 ≥ 0.999, LOD ≤ 0.3 ng mL-1, and RSD ≤ 1.7 % (n = 7). HBCD was not stable under our migration conditions and was not detected in any FCA, food or food simulant, including positive controls. Phenolic BFRs (TBP and TBBPA) migrated at concentrations ranging from non-detected to 73 µg kg-1 in food simulants, and from 1 to 23 µg kg-1 in food. Phenolic BFRs migrated into 50% ethanol food simulant at higher concentrations than in more aqueous food simulants and foods.

Brominated flame retardants (BFRs) in contaminated food contact articles: identification using DART-HRMS and GC-MS.

Any food contact material (FCM) must be approved by the US FDA as being compliant with Title 21 of the Code of Federal regulations Parts 170-199, and/or obtain a non-objection letter through the Food Contact Notification Process, before being placed into the United States market. In the past years, several scientific articles identified FCM or more specifically, food contact articles (FCAs), which were contaminated with brominated flame retardants (BFRs) in the European Union. Prior research has suggested the source of BFR contamination was likely poorly recycled plastics containing waste electrical and electronic equipment (WEEE). We conducted a retail survey to evaluate the presence of BFR-contaminated reusable FCA in the US market. Using a Direct Analysis in Real Time ionisation High-Resolution Mass Spectrometry (DART-HRMS) screening technique and extraction gas chromatography-mass spectrometry (GC-MS) confirmation we were able to identify BFRs present in retail FCAs. Among non-targeted retail samples, 4 of 49 reusable FCAs contained 1-4 BFRs each. The identified BFRs, found in greatest estimated concentrations, were 2,4,6-tribromophenol (TBP), 3,3',5,5'-tetrabromobisphenol A (TBBPA), hexabromocyclododecane (HBCD), decabromodiphenylethane (DBDPE) and decabromodiphenylether (BDE-209). A second targeted FCA sampling (n = 28) confirmed these BFRs persisted in similar articles. Combined sample sets (n = 77) estimated DART false-positive/negative incidences of 5% & 4%, respectively, for BFR screening of FCAs. Because the presence of BFRs in some contaminated FCAs has been demonstrated and since these compounds are possible migrants into food, further studies are warranted. In order to estimate the potential exposure of the identified BFRs and conduct corresponding risk assessments, the next and logical step will be to study the mass transfer of BFRs from the contaminated FCM into food simulants and food.

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. METHODS: A DART ion source coupled to a quadrupole Orbitrap (high-resolution (HR) mass spectrometer) was employed for this study. Ten types of PA polymers and four retail samples were evaluated. The DART-HRMS data for these samples, as well as the DART-MS/MS (MS2 ) data for PA6 and PA66, were obtained, and their repeatability was assessed across days/calibrations, operators, and equipments. RESULTS: Ions corresponding to the cyclic or linear monomers and oligomers of each PA polymer were detected in each DART-HR mass spectrum. Although similar DART-HR mass spectra were obtained for PA6, PA66, and PA6/PA66 (polymer blends of PA6 and PA66), their DART tandem mass spectra were completely different. The analysis was repeatable, and nearly identical DART tandem mass spectra were obtained on different days, by different operators, and with different equipment. This technique was successfully applied to commercially available samples. CONCLUSIONS: Ten types of PA polymers were distinguished using DART-HRMS and DART-MS2 , and their identification using these techniques was straightforward as the characteristic ions for each PA polymer were identified and detected. Furthermore, the spectra were obtained rapidly. Therefore, DART-HRMS can be considered an efficient screening technique for the rapid identification and differentiation of PA polymers.

Assessment of the Impact of Accelerated Migration Testing for Coated Food Cans Using Food Simulants.

In this study, an accelerated migration test on food can coatings into food simulants was investigated. Food simulants covering a wide range of polarity were used to conduct migration tests at 60 °C with storage times ranging from 4 h to 30 days. Epoxy-resins, acrylic-phenolic, polyester, and vinyl coatings were exposed to water, 3% acetic acid, 50% ethanol, and Miglyol 812®. Using liquid chromatography coupled to a variety of detectors (UHPLC-Q-Orbitrap-MS, UFLC-MS/MS, and HPLC-DAD), migration of several monomers and previously identified oligomers, as well as some unidentified migrants, were determined during the experiment. The data from this study was compared to our findings from previous long-term migration studies with storage times ranging from 24 h to 540 days at 40 °C using the same can coating applications. The results illustrate that performing migration experiments for short time periods at 60 °C may mimic migration results that would be obtained at 40 °C after long-term migration tests (up to 1.5 years) from food can coatings into food simulants.

Investigation of the primary plasticisers present in polyvinyl chloride (PVC) products currently authorised as food contact materials.

PVC is a common food contact material that is usually plasticised to increase its flexibility. Phthalates are one class of chemical compounds that are often used as plasticisers in PVC in a wide range of industries. They may be used in packaging materials for foods and can also be found in components of certain food processing equipment such as conveyor belts and tubing. Transfer of plasticisers from packaging to foods can occur. In recent years, there has been increased interest in understanding the health effects of phthalates, as well as the possible human exposure levels. However, there is limited information available about the routes of exposure to phthalates. In July 2014, the Chronic Hazard Advisory Panel (CHAP) produced a report for the U.S. Consumer Product Safety Commission detailing the potential health hazards of phthalates and phthalate alternatives. This report listed diet as one factor contributing greater than or equal to 10% of total phthalate exposure. As a result of this report, the U.S. Food and Drug Administration (FDA) is interested in determining the types of the primary plasticiser present in food packaging and processing materials as well as their concentrations. An investigation was conducted of 56 different samples of PVC food packaging and food processing materials available in the US market using a solvent extraction and GC-MS analysis. Nine different plasticisers including three phthalates, di(2-ethylhexyl) phthalate, diisononyl phthalate and diisodecyl phthalate, were identified in the products tested. The plasticiser concentrations ranged from 1 to 53% depending on the types of food contact materials and the type of plasticiser. Overall, it appears that manufacturers are switching away from phthalates as their primary plasticiser to alternate compounds such as ESBO, ATBC, DEHT, DINCH, DEHA and DINA.

Investigation into perfluoroalkyl substances (PFASs) in a cranberry bog: method development and sampling results.

The contamination of groundwater and surface water from previous uses of perfluoroalkyl substances (PFASs), particularly products containing the contaminants perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA), has become a concern for drinking water and as a potential exposure route to the food supply. In 2016, the Food and Drug Administration (FDA) was asked to investigate a bog in Massachusetts where the surface water was believed to be contaminated with PFASs. As a result, a method was developed for the analysis of PFASs in cranberries, and water and fruit from the affected bog were evaluated. A QuEChERS method was developed and validated for PFOA, PFOS, and six additional shorter-chain PFASs. Method recoveries ranged from 60% to 115% for validation spikes performed at 10, 20 and 40 ng g-1 and method detection limits ranged from 0.2 to 5.6 ng g-1. Bog water samples were analysed using Environmental Protection Agency (EPA) method 537 for PFOA, PFOS and four additional short-chain PFASs. Surface water concentrations for PFOS ranged from 16 to 122 ng L-1 and input water concentrations were 132 ng L-1 and 206 ng L-1. Of the eight water samples, seven had water concentrations that exceeded the EPA health advisory level for PFOS of 70 ng L-1. Of the 42 cranberry samples analysed, none had detects of PFOA or PFOS above their method detection limits (0.4 and 0.5 ng g-1, respectively), nor any of the other short-chain PFASs.

Evaluation of Short-Term and Long-Term Migration Testing from Can Coatings into Food Simulants: Epoxy and Acrylic-Phenolic Coatings.

Traditionally, migration testing during 10 days at 40 °C has been considered sufficient and appropriate for simulating the potential migration of substances from food-contact materials into foods. However, some packages, such as food cans, may be stored holding food for extended time periods (years). This study attempts to verify whether common testing conditions accurately estimate long-term migration. Two types of can coatings, epoxy and acrylic-phenolic, were subjected to short-term and long-term migration testing (1 day-1.5 years) using food simulants (water, 3% acetic acid, 50% ethanol, and isooctane) at 40 °C. Using HPLC-DAD/CAD, HPLC-MS, UHPLC-HRMS (where HRMS is accurate mass, mass spectrometry), and DART-HRMS, we identified potential migrants before starting the experiment: BPA, BADGE, BADGE derivatives, benzoguanamine, and other relevant marker compounds. During the experiment using a water-based food simulant, migrants remained stable. Most of the cans in contact with 3% acetic acid did not survive the experimental conditions. Tracked migrants were not detected in isooctane. In the presence of 50% ethanol, the traditional migration test during 10 days at 40 °C did not predict migration during long-term storage. These results suggest that migration protocols should be modified to account for long-term storage.

A Collaborative Study: Determination of Mycotoxins in Corn, Peanut Butter, and Wheat Flour Using Stable Isotope Dilution Assay (SIDA) and Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS).

A collaborative study was conducted to evaluate stable isotope dilution assay (SIDA) and LC-MS/MS for the simultaneous determination of aflatoxins B1, B2, G1, and G2; deoxynivalenol; fumonisins B1, B2, and B3; ochratoxin A; HT-2 toxin; T-2 toxin; and zearalenone in foods. Samples were fortified with 12 13C uniformly labeled mycotoxins (13C-IS) corresponding to the native mycotoxins and extracted with acetonitrile/water (50:50 v/v), followed by centrifugation, filtration, and LC-MS/MS analysis. In addition to certified reference materials, the six participating laboratories analyzed corn, peanut butter, and wheat flour fortified with the 12 mycotoxins at concentrations ranging from 1.0 to 1000 ng/g. Using their available LC-MS/MS platform, each laboratory developed in-house instrumental conditions for analysis. The majority of recoveries ranged from 80 to 120% with relative standard derivations (RSDs) <20%. Greater than 90% of the average recoveries of the participating laboratories were in the range of 90-110%, with repeatability RSDr (within laboratory) < 10% and reproducibility RSDR (among laboratory) < 15%. All Z scores of the results of certified reference materials were between -2 and 2. Using 13C-IS eliminated the need for matrix-matched calibration standards for quantitation, simplified sample preparation, and achieved simultaneous identification and quantitation of multiple mycotoxins in a simple LC-MS/MS procedure.

Identification of unknown compounds from polyester cans coatings that may potentially migrate into food or food simulants.

Cross-linked polyester resins are being introduced into the market as alternatives to epoxy resins as coatings for metal food cans. Identification of potential migrants, from these coatings into food, is a significant analytical challenge due to the diversity of substances employed in the manufacture of the coatings. However, such identification is required to assess migration from the can coating into the food and quantify dietary exposure. Polyester can coatings were extracted with acetonitrile at 40°C for 24h and the extracts were analyzed by a variety of analytical techniques, including GC-MS, HPLC-DAD/MS, HPLC-DAD/CAD and UHPL C-HRMS. Twenty nine non-volatile oligomers were tentatively identified using retention times, UV spectra, and accurate mass measurements. Identified oligomers suggest the coating in use for food cans is a polyester coating and is mainly based on the monomers isophthalic acid, terephthalic acid and nadic acid. To give confidence in the identification, one of the tentatively identified oligomer was synthetized and analyzed by (13)C and (1)H NMR and UHPL C-HRMS. The NMR and HRMS results, confirmed the presence of this compound in the can extracts. Finally, to determine if rapid, direct detection of the oligomers was practical, the coatings were analyzed by DART-HRMS. Twenty three out of the 29 oligomers were identified in the coating by direct measurement with DART-HRMS in few minutes.

Evaluation of Long-Term Migration Testing from Can Coatings into Food Simulants: Polyester Coatings.

FDA guidance for food contact substances recommends that for food packaging intended for use at sterilized, high temperature processed, or retorted conditions, a migration test with a retort step at 121 °C for 2 h followed by a 10 day migration test at 40 °C should be performed. These conditions are in intended to simulate processing and long-term storage. However, can coatings may be in contact with food for years, and there are very few data evaluating if this short-term testing accurately simulates migration over extended time periods. A long-term migration test at 40 °C with retorted and non-retorted polyester cans using several food simulants (water, 3% acetic acid, 10% ethanol, 50% ethanol, and isooctane) was conducted to verify whether traditional migration testing protocols accurately predict migration from food contact materials used for extended time periods. Time points were from 1 day to 515 days. HPLC-MS/MS was used to analyze polyester monomers, and oligomer migration was monitored using HPLC-DAD/CAD and HPLC-MS. Concentrations of monomers and oligomers increased during the migration experiments, especially in ethanol food simulants. The data suggest that current FDA migration protocols may need to be modified to address changes in migrants as a result of long-term storage conditions.

Target and non-target analysis of migrants from PVC-coated cans using UHPLC-Q-Orbitrap MS: evaluation of long-term migration testing.

A simple, rapid and sensitive method for analyzing multi-target and non-target additives in polyvinyl chloride (PVC) food can coatings using ultra-high-performance liquid chromatography coupled to quadrupole-orbital ion-trap mass spectrometry was developed. This procedure was used to study the behaviour of a cross-linking agent, benzoguanamine (BGA), two slip agents, oleamide and erucamide, and 18 other commonly used plasticisers including phthalates, adipates, sebacates, acetyl tributyl citrate and epoxidised soybean or linseed oils. This optimised method was used to detect these analytes in food simulants (water and 3% acetic acid) in a long-term migration test of PVC-coated food cans for a period ranging from 1 day to 1.5 years at 40°C. Although very low detection limits (5 ng ml(-1)) were obtained for the majority of compounds, none of the monitored plasticisers and slip agents was detected in simulants extracted from cans over the period of the test. However, the presence of BGA in both aqueous food simulants was confirmed based on high-resolution mass spectrometry, product ion spectra and analysis of a reference standard. The BGA concentration in both simulants continued to increase with storage time: after 1.5 years storage in aqueous food simulants at 40°C, BGA was detected at concentrations up to 84 µg dm(-2). We believe this is the first study describing the long-term migration capacity of BGA from any vinyl coating material intended for use in PVC-coated food cans. Our results may have implications for migration test protocols for food cans that will be stored for extended time periods.

Characterisation and potential migration of silver nanoparticles from commercially available polymeric food contact materials.

The potential for consumer exposure to nano-components in food contact materials (FCMs) is dependent on the migration of nanomaterials into food. Therefore, characterising the physico-chemical properties and potential for migration of constituents is an important step in assessing the safety of FCMs. A number of commercially available food storage products, purchased domestically within the United States and internationally, that claim to contain nanosilver were evaluated. The products were made of polyethylene, polypropylene and polyphenylene ether sulfone and all contained silver (0.001-36 mg kg(-1) of polymer). Silver migration was measured under various conditions, including using 3% acetic acid and water as food simulants. Low concentrations (sub-ppb levels) of silver were detected in the migration studies generally following a trend characterised by a surface desorption phenomenon, where the majority of the silver migration occurred in the first of three consecutive exposures. Silver nanoparticles were not detected in food simulants, suggesting that the silver migration may be due solely to ionic silver released into solution from oxidation of the silver nanoparticle surface. The absence of detectable silver nanoparticles was consistent with expectations from a physico-chemical view point. For the products tested, current USFDA guidance for evaluating migration from FCMs was applicable.

Suitability of polystyrene as a functional barrier layer in coloured food contact materials.

Functional barriers in food contact materials (FCMs) are used to prevent or reduce migration from inner layers in multilayer structures to food. The effectiveness of functional barrier layers was investigated in coloured polystyrene (PS) bowls due to their intended condition of use with hot liquids such as soups or stew. Migration experiments were performed over a 10-day period using USFDA-recommended food simulants (10% ethanol, 50% ethanol, corn oil and Miglyol) along with several other food oils. At the end of the 10 days, solvent dyes had migrated from the PS bowls at 12, 1 and 31,000 ng cm(-)(2) into coconut oil, palm kernel oil and Miglyol respectively, and in coconut oil and Miglyol the colour change was visible to the human eye. Scanning electron microscope (SEM) images revealed that the functional barrier was no longer intact for the bowls exposed to coconut oil, palm kernel oil, Miglyol, 10% ethanol, 50% ethanol and goat's milk. Additional tests showed that 1-dodecanol, a lauryl alcohol derived from palm kernel oil and coconut oil, was present in the PS bowls at an average concentration of 11 mg kg(-1). This compound is likely to have been used as a dispersing agent for the solvent dye and aided the migration of the solvent dye from the PS bowl into the food simulant. The solvent dye was not found in the 10% ethanol, 50% ethanol and goat's milk food simulants above their respective limits of detection, which is likely to be due to its insolubility in aqueous solutions. A disrupted barrier layer is of concern because if there are unregulated materials in the inner layers of the laminate, they may migrate to food, and therefore be considered unapproved food additives resulting in the food being deemed adulterated under the Federal Food Drug and Cosmetic Act.

A novel method for the simultaneous determination of 14 sweeteners of regulatory interest using UHPLC-MS/MS.

An improved, efficient, sensitive method for the determination of 14 non-nutritive sweeteners in food products was developed using electrospray ionisation (ESI) ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in the negative-ion mode. Fourteen sweeteners and three internal standards were separated on a reversed-phase UHPLC column using a simple gradient programme. Analyte quantitation and confirmation were performed with data collection in multiple reaction monitoring (MRM) mode. Limits of detection (LODs) were determined in a representative drink, candy and yogurt sample and ranged from 0.1 to 1.8 ng ml(-1) (drinks) and from 0.1 to 2.5 ng g(-1) (candy and yogurt). Repeatability at the limit of quantitation (LOQ) ranged from 1% to 13% relative standard deviation (RSD). Twenty-seven commercially available food products were tested using the optimised method showing that the majority of products contained sweetener concentrations below their assigned maximum usable dose. Recovery studies were performed and accuracy data are presented.