Combination of Structure Databases, In Silico Fragmentation, and MS/MS Libraries for Untargeted Screening of Non-Volatile Migrants from Recycled High-Density Polyethylene Milk Bottles.

Chemical contamination is one of the major obstacles for mechanical recycling of plastics. In this article, we built and open-sourced an in-house MS/MS library containing more than 500 plastic-related chemicals and developed mspcompiler, an R package, for the compilation of various libraries. We then proposed a workflow to process untargeted screening data acquired by liquid chromatography high-resolution mass spectrometry. These tools were subsequently employed to data originating from recycled high-density polyethylene (rHDPE) obtained from milk bottles. A total of 83 compounds were identified, with 66 easily annotated by making use of our in-house MS/MS libraries and the mspcompiler R package. In silico fragmentation combined with data obtained from gas chromatography-mass spectrometry and lists of chemicals related to plastics were used to identify those remaining unknown. A pseudo-multiple reaction monitoring method was also applied to sensitively target and screen the identified chemicals in the samples. Quantification results demonstrated that a good sorting of postconsumer materials and a better recycling technology may be necessary for food contact applications. Removal or reduction of non-volatile substances, such as octocrylene and 2-ethylhexyl-4-methoxycinnamate, is still challenging but vital for the safe use of rHDPE as food contact materials.

Migration of contaminants from printed masks for children to saliva simulant using liquid chromatography coupled to ion mobility-time of flight-mass spectrometry and gas chromatography-mass spectrometry.

The COVID-19 pandemic has led to children using polymeric FFP2 and polymeric surgical masks on a daily basis. Children often bite and suck on such masks as they wear them closed to their mouths. In this work, the migration of contaminants from printed and unprinted children`s masks to a saliva simulant has been studied. Liquid chromatography coupled to ion-mobility quadrupole time-of-flight mass spectrometry has been used for the detection and identification of non-volatile migrants. An orthogonal projection to latent structures - discriminant analysis (OPLS-DA) was applied to compare the data from the printed masks against the data from the unprinted ones. Headspace solid phase microextraction coupled to gas chromatography mass spectrometry was used to assess the migration of volatile compounds. Thirteen compounds were found in the masks with concentrations ranging from 5 ng/g to 254 ng/g. Toluene, chlorobenzene, irganox 1076 and 2-(2-butoxyethoxy)ethyl acetate were all found to migrate from the masks studied. Moreover, differences between the migrants from printed and unprinted FFP2 masks were found. Octocrylene, 4-(dimethylamine)benzoate, methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate and tris(3-methylphenyl)phosphate were found to migrate only from printed masks. Toluene that migrated from all the masks studied and tris(3-methylphenyl)phosphate, that migrated only from printed masks, have been listed as hazardous priority substances.

Non-invasive oxygenation support in acutely hypoxemic COVID-19 patients admitted to the ICU: a multicenter observational retrospective study.

BACKGROUND: Non-invasive oxygenation strategies have a prominent role in the treatment of acute hypoxemic respiratory failure during the coronavirus disease 2019 (COVID-19). While the efficacy of these therapies has been studied in hospitalized patients with COVID-19, the clinical outcomes associated with oxygen masks, high-flow oxygen therapy by nasal cannula and non-invasive mechanical ventilation in critically ill intensive care unit (ICU) patients remain unclear. METHODS: In this retrospective study, we used the best of nine covariate balancing algorithms on all baseline covariates in critically ill COVID-19 patients supported with > 10 L of supplemental oxygen at one of the 26 participating ICUs in Catalonia, Spain, between March 14 and April 15, 2020. RESULTS: Of the 1093 non-invasively oxygenated patients at ICU admission treated with one of the three stand-alone non-invasive oxygenation strategies, 897 (82%) required endotracheal intubation and 310 (28%) died during the ICU stay. High-flow oxygen therapy by nasal cannula (n = 439) and non-invasive mechanical ventilation (n = 101) were associated with a lower rate of endotracheal intubation (70% and 88%, respectively) than oxygen masks (n = 553 and 91% intubated), p < 0.001. Compared to oxygen masks, high-flow oxygen therapy by nasal cannula was associated with lower ICU mortality (hazard ratio 0.75 [95% CI 0.58-0.98), and the hazard ratio for ICU mortality was 1.21 [95% CI 0.80-1.83] for non-invasive mechanical ventilation. CONCLUSION: In critically ill COVID-19 ICU patients and, in the absence of conclusive data, high-flow oxygen therapy by nasal cannula may be the approach of choice as the primary non-invasive oxygenation support strategy.

Direct Immersion-Solid-Phase Microextraction Coupled to Gas Chromatography-Mass Spectrometry and Response Surface Methodology for Nontarget Screening of (Semi-) Volatile Migrants from Food Contact Materials.

Toward a more rigorous inspection of food contact materials, the importance of sample preparation for nontarget screening should be addressed. Direct immersion-solid-phase microextraction coupled to gas chromatography mass spectrometry (DI-SPME-GC-MS) was optimized for nontarget screening of migrants in 3% acetic acid, 10% ethanol, and 95% ethanol food simulants by response surface methodology (RSM) in the present study. Optimum conditions were DVB/CAR/PDMS fiber, no pH adjustment for 10% and 95% ethanol simulant but pH adjustment to 7 for 3% acetic acid simulant, no salt addition, 5 min preincubation, 55 min extraction at 70 °C, and 8 min desorption at 250 °C. In addition, 9.5 times dilution of 95% ethanol samples prior to extraction was required. pH modification of 3% acetic acid samples was found to be critical for the extraction of amines. The proposed methodology was then evaluated by determining the limit of detection (LOD) as well as repeatability of 35 food contact materials-related substances. Except for those amines and diols which have a relatively high LOD, the LODs of the rest of the substances were 0.1-14.1 µg/kg with a precision of 1.9-23.0% in 10% ethanol and were 0.1-20.2 µg/kg with a precision of 2.5-19.6% in 3% acetic acid simulant. The LOD and precision in 95% ethanol simulant were 0.7-163.7 µg/kg and 1.4-26.8%, respectively. The proposed method can be applied for an overall screening of migrants from these three simulants at even trace levels, though attention should be paid to some specific analytes, e.g., diols and amines, which could have a high LOD and toxicity.

Influence of nonylphenol from multilayer plastic films on artificial insemination of sows.

Artificial insemination is common practice in mass livestock farming. Recently, it was shown that chemicals leaching from multilayer plastic bags affect the fertility of boars, although common quality tests did not show any impact on the sperm. It is not clear whether this incidence was a single case or whether it could be a systematic problem. Therefore, we studied six multilayer plastic bags. A total of 49 compounds were found, but most of them were at very low intensity. Nonylphenols in the range of 19-99 µg/g plastic were found. Migration tests using water and 10% ethanol as simulants, to mimic the behavior of semen with the extender, were performed. The most interesting migrants in terms of potential reprotoxicity were identified as nonylphenols. The identification in depth demonstrated the presence of 10 isomers of nonylphenol with a total concentration range between 16 to 58 µg/Kg simulant, among other migrants at lower concentration. The influence of these nonylphenols and their maximum tolerable concentration in direct contact with semen from boars was studied. Motility, viability, mitochondrial activity and acrosomes reacted were significantly affected at 10 mg/Kg of nonylphenols in contact with the sperm, but in vitro penetration rate was significantly decreased with only 2 mg/Kg. Insight into the mode of action is also provided.

Ion-Mobility Quadrupole Time-of-Flight Mass Spectrometry: A Novel Technique Applied to Migration of Nonintentionally Added Substances from Polyethylene Films Intended for Use as Food Packaging.

Nontarget analysis of nonvolatile substances in complex samples is a very challenging task that requires powerful analytical techniques and experience of analyzing such samples. An extensive study was conducted in order to identify nonintentionally added substances (NIAS) migrating from 18 polyethylene (PE) samples intended to be in contact with food. The migration assays were performed in five simulants and analyzed by ultrahigh-performance liquid chromatography (UPLC) coupled to an ion-mobility separation (IMS) quadrupole-time-of-flight (QTOF) mass spectrometer. This experimental setup provides a novel and powerful tool for this type of nonvolatile and nontargeted analysis. Thirty-five compounds were identified, 17 of which were NIAS. Methyl and ethyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoate were found to be degradation products of either Irganox 1010 or Irganox 1076. Additionally, breakdown products including hexa-heptadecanamide, N,N'-1,2-ethanediylbis- and 11-eicosenamide were identified together with impurity reaction products, e.g., dibutyl amine or compounds of unknown origin like phosphine oxide, tributyl-. Forty-five percent of the detected compounds are in the positive list contained in Regulation 10/2011/EU, and their migration values were below their specific migration limits. The risk assessment for the rest of the compounds was carried out by comparing their migration values to the maximum concentration recommended by Cramer, e.g., ethyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoate and benzenepropanoic acid, 3,5-bis(1,1-dimethylethyl)-4-hydroxy-, 1,1'-[2,2-bis(hydroxymethyl)-1,3-propanediyl] ester (both class II toxicity), heptadecanamide, N,N'-1,2-ethanediylbis-, and phosphine oxide, tributyl- (both class III toxicity) were above the maximum concentration values for three samples that were migrated to ethanol 95%, and therefore, these samples are not suitable for food contact. The analytical tools and procedures used in this study are presented and discussed in detail.

Nano selenium as antioxidant agent in a multilayer food packaging material.

Selenium nanoparticles (SeNPs) were incorporated in a flexible multilayer plastic material using a water-base adhesive as vehicle for SeNPs. The antioxidant performance of the original solutions containing spherical SeNPs of 50-60 nm diameter, the adhesive containing these SeNPs, and the final multilayer plastic material to be used as food packaging were quantitatively measured. The radical scavenging capacity due to SeNPs was quantified by a free radical assay developed in the laboratory and by the diphenyl-1-picrylhydrazyl (DPPH) method. DPPH was not efficient to measure the scavenging capacity in the multilayer when the free radical scavenger is not in the surface in contact with it. Several multilayer laminated structures composed by [PET (20 m)-adhesive-LDPE (with variable thickness from 35 to 90 µm)] were prepared and measured, demonstrating for the first time that free radicals derived from oxygen (OH·, O2·, and O2H) cross the PE layer and arrive at the adhesive. SeNPs remain as such after manufacture and the final laminate is stable after 3 months of storage. The antioxidant multilayer is a non-migrating efficient free radical scavenger, able to protect the packaged product versus oxidation and extending the shelf life without being in direct contact with the product. Migration tests of both Se and SeNPs to simulants and hazelnuts demonstrated the non-migrating performance of this new active packaging. Graphical abstract ᅟ.

UPLC-ESI-Q-TOF-MS(E) and GC-MS identification and quantification of non-intentionally added substances coming from biodegradable food packaging.

Biodegradable packagings are made by combination of several materials creating a multilayer with the properties needed. Each material, including the adhesive, could contain substances that could migrate to the food. In this work, gas chromatography coupled with mass spectrometry and ultra-high-pressure liquid chromatography coupled with quadrupole time-of-flight mass spectrometry were used to identify the biodegradable adhesive compounds. Five of the 13 compounds identified were nonintentionally added substances; they were neoformed compounds created by the reaction of added compounds in the adhesive. Moreover, the migration of the compounds through four different biodegradable materials-paper, polylactic acid, ecovio®, and polyvinyl alcohol-was studied for the first time. Three of the 13 compounds identified in the adhesive migrated from the adhesive to Tenax®, which was used as a solid food simulant. One of them, 2,4,7,9-tetramethyl-5-decyne-4,7-diol, was an intentionally added substance, and the other two were 1,6-dioxacyclododecane-7,12-dione and 1,6,13,18-tetraoxacyclotetracosane-7,12,19,24-tetraone, which were nonintentionally added substances identified in this work. Higher migration values (ranging from 0.81 to 2.07 mg/kg) were observed for migration through ecovio® than through the multilayer made by combination of ecovio® and polyvinyl alcohol (0.07-0.39 mg/kg) owing to the barrier effect provided by polyvinyl alcohol. The migration values for migration through paper and polylactic acid were below the limits of detection.

Relationship between volume and survival in closed intensive care units is weak and apparent only in mechanically ventilated patients.

BACKGROUND: Recent studies have found an association between increased volume and increased intensive care unit (ICU) survival; however, this association might not hold true in ICUs with permanent intensivist coverage. Our objective was to determine whether ICU volume correlates with survival in the Spanish healthcare system. METHODS: Post hoc analysis of a prospective study of all patients admitted to 29 ICUs during 3 months. At ICU discharge, the authors recorded demographic variables, severity score, and specific ICU treatments. Follow-up variables included ICU readmission and hospital mortality. Statistics include logistic multivariate analyses for hospital mortality according to quartiles of volume of patients. RESULTS: The authors studied 4,001 patients with a mean predicted risk of death of 23% (range at hospital level: 14-46%). Observed hospital mortality was 19% (range at hospital level: 11-35%), resulting in a standardized mortality ratio of 0.81 (range: 0.5-1.3). Among the 1,923 patients needing mechanical ventilation, the predicted risk of death was 32% (14-60%) and observed hospital mortality was 30% (12-61%), resulting in a standardized mortality ratio of 0.96 (0.5-1.7). The authors found no correlation between standardized mortality ratio and ICU volume in the entire population or in mechanically ventilated patients. Only mechanically ventilated patients in very low-volume ICUs had slightly worse outcome. CONCLUSION: In the currently studied healthcare system characterized by 24/7 intensivist coverage, the authors found wide variability in outcome among ICUs even after adjusting for severity of illness but no relationship between ICU volume and outcome. Only mechanically ventilated patients in very low-volume centers had slightly worse outcomes.

Identification of non-volatile compounds and their migration from hot melt adhesives used in food packaging materials characterized by ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

The identification of unknown non-volatile migrant compounds from adhesives used in food contact materials is a very challenging task because of the number of possible compounds involved, given that adhesives are complex mixtures of chemicals. The use of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-MS/QTOF) is shown to be a successful tool for identifying non-targeted migrant compounds from two hot melt adhesives used in food packaging laminates. Out of the seven migrants identified and quantified, five were amides and one was a compound classified in Class II of the Cramer toxicity. None of the migration values exceeded the recommended Cramer exposure values.

The migration of NIAS from ethylene-vinyl acetate corks and their identification using gas chromatography mass spectrometry and liquid chromatography ion mobility quadrupole time-of-flight mass spectrometry.

An exhaustive migration study of eight corks, made of ethylene-vinyl acetate, was carried out to identify any non-volatile and volatile compounds using an untargeted approach. The challenge associated with the structural elucidation of unknowns was undertaken using both ultra-high-performance liquid chromatography coupled to an ion-mobility separation quadrupole-time of flight mass spectrometer and gas chromatography mass spectrometry. A total of fifty compounds were observed to migrate from the corks, and among these additives such as antioxidants (Butyl 4-hydroxybenzoate, Irganox 1010, Irganox 1075, Irgafos 168 and BHT) or lubricants (EBO and octadecanamide, N,N'-1,2-ethanediylbis-) were identified. A high proportion (84%) of the detected compounds was non-intentionally added substances (NIAS), and included several cyclic oligomers with different chain sequences. NIAS, such as 2,6-bis(1,1-dimethylethyl)-4-ethyl and 7,9-ditert-butyl-1-oxaspiro[4.5]deca-6,9-diene-2,8-dione, break-down products, including hexa-, hepta- and nonadecanamide, N,N'-1,2-ethanediylbis-, and oxidation products were also identified. One cork was found to be unsuitable for use as a food contact material.

The detection and elucidation of oligomers migrating from biodegradable multilayer teacups using liquid chromatography coupled to ion mobility time-of-flight mass spectrometry and gas chromatography-mass spectrometry.

Biodegradable materials are increasingly being used in manufacturing processes due to their environmental benefits. In this work, a study has been performed to assess the migration of compounds from biodegradable multilayer teacups to a tea solution. Liquid chromatography in conjunction with ion-mobility quadrupole time-of-flight mass spectrometry has been used for the elucidation of non-volatile compounds. An orthogonal projection to latent structures-discriminant analysis has been carried out to compare the tea after migration against untreated tea used as blank. Headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry has been optimised to analyse the migration of volatile compounds. Eight migrants were identified in the tea, six of which were non-intentionally added oligomers. The degree of migration for hot tea ranged from 0.05 and 4.68 mg/kg, exceeding the specific migration limit. Nevertheless, the migration to cold tea was an order of magnitude lower (between 0.003 and 0.56 mg/kg).

The application of ion mobility time of flight mass spectrometry to elucidate neo-formed compounds derived from polyurethane adhesives used in champagne cork stoppers.

Polyurethane adhesives are used to bond agglomerated cork and natural disk cork to produce cork stoppers that are used in champagne bottles. These adhesives are manufactured by reacting polyols with an excess of diisocyanates. Isocyanates are highly reactive compounds that have a propensity to form non-intentionally added substances (NIAS) in the end product. In this work, ion mobility-time of flight-mass spectrometry was used to elucidate such NIAS, through the comparison of accurate mass spectra with the fragmentation patterns of proposed candidates. Twelve neo-formed compounds, including amines, amides and urethanes, resulting from the reaction of isocyanates with acetic acid and ethanol used as food simulants, were identified. Additionally, markers from champagne vs. champagne after its exposure to the adhesive were investigated using the supervised multivariate analysis method of Orthogonal Projection to Latent Structures - Discriminant Analysis. Four neo-formed compounds, resulting from the reaction of diisocyanates with malic acid or tartaric acid contained in the champagne, were identified for the first time in this work. All of the compounds identified were subsequently quantified using ultra-high pressure liquid chromatography coupled to a triple quadrupole mass spectrometer. Limits of detection were below 5 µg/kg in the food simulants and below 30 µg/kg in champagne samples. Migration levels ranged from 70 to 721 µg/kg, with most of them exceeding the specific migration limit established for Cramer class III compound (90 µg/kg).

Influence of cooking conditions on the migration of silicone oligomers from silicone rubber baking molds to food simulants.

The stability, surface micromorphology, and volatile organic compounds (VOCs) of silicone rubber baking molds (SRBMs) were tested while using the molds under severe conditions: baking at 175 °C, microwaving at 800 W, and freezing at -18 °C. Moreover, migration tests of SRBMs to food simulants (isooctane, 95% ethanol, and Tenax®) at 70 °C for 2 h (accelerated conditions) were performed. The initial total VOCs concentration was 2.53% higher than that recommended by BfR Recommendations on Food Contact Materials. Therefore, the SRBM samples were considered as badly tempered materials, and 18 different types of silicone oligomers were identified during the migration tests. The following percentage of silicone oligomers with a molecular weight lower than 1000 Da in isooctane, 95% ethanol, and Tenax® were detected: 70.7%, 91.8%, and 97.2%, respectively. It has been proven that previous baking treatments effectively reduced the content of silicone oligomers migrating from SRBMs.

The use of ion mobility time-of-flight mass spectrometry to assess the migration of polyamide 6 and polyamide 66 oligomers from kitchenware utensils to food.

Oligomers, are, in general, unknown components of the polymer. These oligomers can migrate from the polymer into the food and become a non-intentionally added substance to the food. In this work, ion mobility time-of-flight mass spectrometry has been used to identify oligomers migrating from kitchenware. The structure elucidation of oligomers from polyamide 6 and polyamide 66 was achieved through the analysis of accurate m/z values of adducts and collision cross section values of precursor ions together with high-energy fragmentation patterns. Additionally, a method to extract oligomers from sunflower oil, cooked beans, soup and whole milk has been developed. Extraction recoveries ranged from 87 to 102% and limits of detection were from 0.03 to 0.11 mg/kg. It was observed that the migration from kitchenware to real food was below the specified migration limit of 5 mg/kg. However, this limit was exceeded for food simulants, which therefore overestimated the oligomer migration.

Long-term survival of mechanically ventilated patients with severe COVID-19: an observational cohort study.

BACKGROUND: Information is lacking regarding long-term survival and predictive factors for mortality in patients with acute hypoxemic respiratory failure due to coronavirus disease 2019 (COVID-19) and undergoing invasive mechanical ventilation. We aimed to estimate 180-day mortality of patients with COVID-19 requiring invasive ventilation, and to develop a predictive model for long-term mortality. METHODS: Retrospective, multicentre, national cohort study between March 8 and April 30, 2020 in 16 intensive care units (ICU) in Spain. Participants were consecutive adults who received invasive mechanical ventilation for COVID-19. Severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) infection detected in positive testing of a nasopharyngeal sample and confirmed by real time reverse-transcriptase polymerase chain reaction (rt-PCR). The primary outcomes was 180-day survival after hospital admission. Secondary outcomes were length of ICU and hospital stay, and ICU and in-hospital mortality. A predictive model was developed to estimate the probability of 180-day mortality. RESULTS: 868 patients were included (median age, 64 years [interquartile range [IQR], 56-71 years]; 72% male). Severity at ICU admission, estimated by SAPS3, was 56 points [IQR 50-63]. Prior to intubation, 26% received some type of noninvasive respiratory support. The unadjusted overall 180-day survival rates was 59% (95% CI 56-62%). The predictive factors measured during ICU stay, and associated with 180-day mortality were: age [Odds Ratio [OR] per 1-year increase 1.051, 95% CI 1.033-1.068)), SAPS3 (OR per 1-point increase 1.027, 95% CI 1.011-1.044), diabetes (OR 1.546, 95% CI 1.085-2.204), neutrophils to lymphocytes ratio (OR per 1-unit increase 1.008, 95% CI 1.001-1.016), failed attempt of noninvasive positive pressure ventilation prior to orotracheal intubation (OR 1.878 (95% CI 1.124-3.140), use of selective digestive decontamination strategy during ICU stay (OR 0.590 (95% CI 0.358-0.972) and administration of low dosage of corticosteroids (methylprednisolone 1 mg/kg) (OR 2.042 (95% CI 1.205-3.460). CONCLUSION: The long-term survival of mechanically ventilated patients with severe COVID-19 reaches more than 50% and may help to provide individualized risk stratification and potential treatments. TRIAL REGISTRATION: ClinicalTrials.gov Identifier: NCT04379258. Registered 10 April 2020 (retrospectively registered).

Compounds responsible for off-odors in several samples composed by polypropylene, polyethylene, paper and cardboard used as food packaging materials.

Seven commercial samples, consisted of plastic bags, tetrabrik and box, were evaluated by gas chromatography-olfactometry-mass spectrometry (GC-O-MS) to find the compounds responsible for off-odors in different PP, PE, multilayer cardboard and paper materials used for food contact. Migration assays were carried out with Tenax as food simulant to analyze the food safety as well as to evaluate the odor intensity after migration assay. Forty six compounds with characteristic odors were directly found in the materials studied. The strongest odors identified were acetic, propanoic and butyric with vinegar and rancid odors and octanal, nonanal and decanal with fat/soup odors, all of them found in PP and PE samples. Trimethylbenzenes with solvent and oily odors as well as terpenes with weakly woody odors were found in cardboard and paper materials. After migration, all compounds were below the European Legislation limits and maximum migration values recommended by Cramer. However propanoic, acetic and butyric acid as well as aldehydes compounds, phenol and 1-octanol were detected by sniffers, after migration assay, with high modified frequency (between 50 and 78%), what could change the organoleptic properties of packaged food.

Ion mobility quadrupole time-of-flight high resolution mass spectrometry coupled to ultra-high pressure liquid chromatography for identification of non-intentionally added substances migrating from food cans.

Sealants, incorporated in the lids of food cans to ensure the can is hermetically sealed, are formulated from a wide variety of compounds. These compounds and associated non-intentionally added substances (NIAS) could migrate to the food contained in the can. In this work, ion mobility quadrupole time-of-flight mass spectrometry coupled to ultra-high performance liquid chromatography (UHPLC-IM-QTOF-MS) has been used to obtain ion mobility filtered extracted ion chromatograms. Subsequently, accurate mass precursor ions and their fragments have been used to identify the compounds migrating from the sealant to the content of the cans. Moreover, the correlation between the collision cross-section (CCS) values and m/z of the compounds was used to increase the level of confidence of the identification. Seven compounds were found to have migrated to the food simulants. The compounds bis(2-hydroxy-3-tert-butyl-5-methylphenyl)dicyclopentane,1-tetradecanesulfonic acid, 1-pentadecanesulfonic acid, 1-hexadecanesulfonic acid and naphthalene-2-sulfonic acid (whose migration was over the specific migration limit established by the European Regulation 10/2011/EU) were identified as NIAS in the food simulants studied.

Migration of dihydroxyalkylamines from polypropylene coffee capsules to Tenax® and coffee by salt-assisted liquid-liquid extraction and liquid chromatography-mass spectrometry.

Migration of N,N-Bis(2-hydroxyethyl) alkyl(C8-C18)amines from five different polypropylene capsules to Tenax® and coffee powder have been studied. A single step extraction-cleanup procedure using salting out liquid-liquid extraction (SALLE) method followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was applied. The critical parameters on the SALLE procedure such as extracting solvent, extracting volume, sample pH, salt and its concentration were optimized. The recovery values were in the range of 87.5%-106.5%. The %RSD were lower than 3.7%. The limit of detection was improved from 2.3 ng/g in Tenax® to 0.8 ng/g in coffee. The results indicated that the analyzed compounds have the potential to migrate from the polypropylene capsule containers to the coffee. In most of the cases, the migrated values were higher in Tenax® than in coffee in a range between 1.8 and 61%. One sample did not comply with the specific migration limit established by the European Commission.