Non-invasive tests are increasingly being used to improve the diagnosis and prognostication of chronic liver diseases across aetiologies. Herein, we provide the latest update to the EASL Clinical ...Practice Guidelines on the use of non-invasive tests for the evaluation of liver disease severity and prognosis, focusing on the topics for which relevant evidence has been published in the last 5 years.
A simple, fast, sensitive and reliable method was developed for the simultaneous determination of 13 food contact materials (FCM) regulated substances and non-intentionally added substances (NIAS) ...migrating into official food simulants. The method has been optimized to quantify the monomers styrene and α-methyl styrene, selected polystyrene oligomers (dimers, trimers) and polyester urethane-based oligomers (PU) cyclic oligomers, as well as cyclic NIAS originating from food packaging such as 2,6-Di-tert-butylbenzoquinone and 7,9-Di-tert-butyl-1-oxaspiro(4,5)deca-6,9-diene-2,8-dione.
The method employs liquid-liquid extraction of aqueous ethanol food simulants with dichloromethane, and analysis with gas chromatography coupled to mass spectrometry (GC-MS) with a total analysis time of less than 16 min, with limits of detections ranging from 0.32 ng mL−1 (1,1-diphenyl-ethylene) to 14.8 ng mL−1 for 7,9-di-tert-butyl-1-oxaspiro4.5deca-6,9-diene-2,8-dione and respective limits of quantification from 1.0 ng mL−1 to 41.7 ng mL−1, for the same analytes.
Accuracy and precision results showed that the method is sufficiently accurate for all target analytes, with recoveries ranging between 80 and 110% and relative standard deviations (RSDs) smaller than 16% at the three selected concentration levels.
The method has been successfully applied to seven FCM. Results indicated that significant amounts of polystyrene monomers, dimers and trimers are migrating into food simulants; this is also the case for polyester urethane-based oligomers (PU). Exposure assessment estimation was performed using EFSA’s approach on the total sum of migrating oligomers. In certain cases, amounts of PS and PU oligomers found to be in some cases higher than the respective limits, for the sum of oligomers with a MW lower than 1000 Da.
Display omitted
Food contact materials (FCM) are defined as the objects and materials intended to come into direct or indirect contact with foodstuff, while food contact articles are defined as objects, being ...equipment, containers, packaging and various utensils which are clearly intended to be used for the manufacture, preparation, conservation, flow, transport or handling of foodstuffs ...
•A fast and sensitive method with simple sample preparation is presented.•Use of multiple reaction monitoring (MRM) acquisition.•Application of deuterated internal standards.•Simple salt-assisted ...liquid–liquid extraction (SALLE).•Applicability of the method to food packaging materials.
A simple and fast method was developed for the simultaneous determination of 75 plastic food contact material (FCM) in liquid food simulants, at levels of a few ng g−1. The method employs an optimised salt-assisted liquid–liquid extraction for all EU-regulated ethanol/H2O food simulants, in the presence of 10% NaCl (simulants A and C) or 5% NaCl (simulant D1), and dichloromethane as the extracting solvent. Gas chromatography with triple-quad MS operating in multiple reaction monitoring acquisition was used, applying isotope dilution with selected deuterated compounds. Adequate sensitivity was demonstrated for all analytes. The results also showed sufficient accuracy for the majority of substances, with recoveries of 70–120% and repeatability (expressed as relative standard deviations, RSDs) smaller than 15%. The method was applied to the analysis of FCM multilayer items after undergoing migration testing according to the specifications of the current EU legislation in force.
•PET cyclic oligomers in food contact materials (teabags).•Application of UHPLC-qTOF-MS for identification of potential migration levels.•Method validation for 1st Series PET cyclic oligomers with ...analytical standards of known purity.•In silico toxicity assessment.•Exposure assessment based on EFSA scientific opinions.
Determination of polyethylene terephthalate (PET) dimer up to heptamer 1st series cyclic oligomers, applying an LC-qTOF-MS method, has been developed and validated. Recoveries ranged between 80 and 112% with RSDs lower than 15%. An innovative semi-quantitative approach has been applied for 2nd and 3rd series cyclic oligomers, using the closest structural-similar 1st series cyclic oligomer standard as analytical reference. Oligomers from the three series were quantified in PET teabags after migration experiments with water and food simulants C (20% v/v ethanol in water) and D1 (50% v/v ethanol in water). No legal migration limits exist currently for these substances. In silico genotoxicity assessment of all identified oligomers has been performed and showed no genotoxicity alert for linear or cyclic molecules. Exposure assessment was performed using EFSA’s approach on the total sum of migrating oligomers and on toxicological threshold-of-concern. Amounts found in water were in some cases significantly higher than the respective limits, especially in the worst-case scenario of multiple consumption.
•Migration testing of food packaging materials.•GC-MS analysis of caprolactam (regulated additive) and 2,4-di-tert-butylphenol (NIAS).•Method application to real food packaging material.•Salinity ...level of food simulants may influence migration of analytes from packaging.
Caprolactam and 2,4-di-tert-butyl phenol (2,4-DTBP) are substances typically found in some food contact materials (FCMs). They are known to often migrate into food, and are difficult to analyse in liquid food simulants using GC. In this work a simple salting-out Liquid-Liquid Extraction (SALLE) for the analysis of both substances in water and the official food simulant A (10 % v/v ethanol, Regulation (EU) No. 10/2011) is presented. The method, which included analytical determination by GC-MS, was optimized and validated to ensure sufficient analytical quality.
The method’s LOQs allowed the proper quantification of caprolactam at its EU legislative limit (15 mg kg−1). For 2,4-DTBP the method also revealed good sensitivity, although no official limits have been established yet. Linear regression coefficients (R2) were in all cases higher than 0.999, and recoveries ranged from 87 % and 95% for caprolactam and 2,4-DTBP, respectively. Precision was also acceptable, with the RSDs (%) below 12 %. The method proved to be adequate to be used for routine analysis.
The presence of salt during migration of caprolactam and 2,4-DTBP was also investigated in this work. Polyamide/polyethylene FCM multilayer films have been tested with water and simulant A, containing different amounts of NaCl (up to 15 % m/v), and applying different migration conditions (temperature and time). The results indicated that salinity plays an important effect on the migration of caprolactam, with the presence of salt reducing its migration in case of water and increasing it in case of simulant A. These preliminary results seem to indicate that migration testing should consider not only the well-known fatty content of a food, but also its salinity content, as it may end up affecting drastically the migration of polar substances.
Chemical substances shall not migrate from food contact materials (FCM) at levels that are potentially harmful for the consumers. Each of the current analytical methods applied to verify the ...migration of substances from FCM covers only one or few substances. There is a very limited number of publications on the development of analytical methods allowing the simultaneous determination of several classes of FCM substances, and almost none of them reported methods entirely dedicated to the ones in the positive list of Commission Regulation (EU) No. 10/2011 for plastic FCMs. Therefore, a simple, sensitive and reliable multi-analyte method was developed for the analysis of FCM substances in food simulants. It employs an optimised liquid-liquid extraction with dichloromethane as extraction solvent in the presence of 10% m/v NaCl, followed by quantitative analysis with gas chromatography coupled to mass spectrometry (GC-MS). A combination of total ion chromatograms (TICs) and extracted ion chromatograms (EICs) was used. The optimisation and validation of the method have been carried out according to current international guidelines. Adequate sensitivity was demonstrated in the selected concentration ranges for most of the analytes, with limits of quantification (LOQs) at least three times lower than the legislative limit, when existing. The results showed that the method is sufficiently accurate for the majority of substances, with recoveries between 70 and 115% and relative standard deviations (RSDs) smaller than 20% at three concentration levels. The method was applied to the analysis of some FCM multilayers. The method allows, for the first time, the simultaneous quantification of 84 FCM substances in two of the official food simulants (A and C) at levels of a few ng g
−1
.
Graphical abstract
•PET and PBT cyclic oligomers in food contact materials (plastic coffee capsules).•Validation and application of a HPLC-UV/FLD for quantification of the studied PET and PBT oligomers.•Method ...validation for 1st Series PET cyclic oligomers and PBT, with proper analytical standards, with known purity.•Exposure assessment based on TTC and EFSA scientific opinions.
A HPLC-UV/FLD method was validated for the quantification of six polyethylene terephthalate (PET) and four polybutylene terephthalate (PBT) oligomers. PBT oligomers are EU regulated, while the PET ones are considered non-intentionally added substances (NIAS). LOQs were higher than 0.4 and 3.5 μg kg−1 for the simulants and in the polymer extracts, respectively. Recoveries ranged from 95 to 114 % with RSDs below 12%. Migration testing of PBT and polypropylene coffee capsules were performed with H2O and simulant C, and extracts were obtained with accelerated solvent extraction (ASE). For the latter legislative limits weren’t surpassed. As no migration limits are existing for the analytes, both EFSA’s toxicological threshold of concern (TTC) and sum of oligomers approaches were applied. The majority of oligomers were below the TTC (90 µg/person/day), but the limit value of 50 µg/kg food was surpassed for some capsules, which indicates a significant intake in both single and multiple consumption.
Summary
Serum ferritin level is one of the most commonly requested investigations in both primary and secondary care. Whilst low serum ferritin levels invariably indicate reduced iron stores, raised ...serum ferritin levels can be due to multiple different aetiologies, including iron overload, inflammation, liver or renal disease, malignancy, and the recently described metabolic syndrome. A key test in the further investigation of an unexpected raised serum ferritin is the serum transferrin saturation. This guideline reviews the investigation and management of a raised serum ferritin level. The investigation and management of genetic haemochromatosis is not dealt with however and is the subject of a separate guideline.
•Migrating compounds of polysaccharide-films were identified by UHPLC-TIMS-TOF-MS.•Monoacetylated maltose migrated from acetylated starch at 70 °C/2 h with lipophilic simulant.•Dibutyl phthalate ...(DBP) migrated from all biopolymers at high temperature/short time.•No in silico toxicity alert was identified for the migrating compounds.•Organocatalytic acetylated FCM biopolymers did not show any safety concern.
The chemical safety of representative polysaccharide films made with pea starch, organocatalytic acetylated pea starch and pectin was investigated at different migration conditions (20 °C/10 days, 70 °C/2 h) using two official simulants signifying hydrophilic (simulant A, 10% ethanol) or lipophilic (simulant D1, 50% ethanol) foods. Migrating semi-volatile and non-volatile compounds were identified and semi-quantified by ultra-high performance liquid chromatography-trap ion mobility time-of-flight mass spectrometry (UHPLC-TIMS-TOF-MS/MS), whereas their toxicity was evaluated by in silico models based on qualitative structure activity (QSAR). Physicochemical analysis revealed polymer wash-off into the simulants. Migration testing at 70 °C for 2 h using simulant D1 resulted in detectable concentrations of glycerol (≤72.1 mg/kg), monoacetylated maltose (≤6.5 mg/kg), and dibutyl phthalate (DBP) (≤0.5 mg/kg, compliant with the existing legislative migration limits) in samples containing acetylated starch. Migrating 3-β-galactopyranosyl glucose (≤8.9 mg/kg) and 2,5-diketo-d-gluconic acid (≤4.9 mg/kg) were detected at 20 °C/10 days. In-silico toxicity emphasized no significant toxicity and categorized organocatalytic acetylated pea starch of no safety concern.
PDF
