Screening of 152 Veterinary Drug Residues in Animal Source Foods by LC-MS/MS, Multilaboratory Validation Study: Final Action 2020.04.

BACKGROUND: The presence of veterinary drug residues in food-producing animals and animal products is regulated through the enforcement of maximum residue limits (MRLs). To answer the need of the food sector to monitor these substances in a wide range of food commodities, stakeholders at AOAC identified the need for a reliable confirmatory screening method. Such qualitative approach is required for compliance checking and to support product release in manufacturing. OBJECTIVE: Data were collected from 5 independent laboratories that applied the AOAC Official First Action Method AOAC 2020.04 to demonstrate adequate performance under reproducibility conditions. Probability of Detection (POD) was calculated in blank test samples and test samples spiked at the Screening Target Concentration (STC) level, with the objective to achieve PODs ≤ 10% and ≥ 90%, respectively. Additionally, the effectiveness of the screening method was assessed through participation to 92 proficiency test samples. METHODS: Four streams were optimized to screen for 152 veterinary drug residues by LC-MS/MS in a wide variety of food commodities including milk-based ingredients and related products (e.g., milk fractions, infant formula, infant cereals and baby foods), meat- and fish-based ingredients and related products (fresh, powdered, cooked, infant cereals and baby foods) and other ingredients such as eggs, animal fat and animal byproducts. The four streams covered 105 antibiotic residues, anti-inflammatory and antiparasitic agents (Stream A); 23 Beta-lactams (Stream B); 14 Aminoglycosides (Stream C) and 10 Tetracyclines (Stream D). RESULTS: The multi-laboratory validation led to PODs at the STC ≥ 94% and PODs in the blank ≤ 9%. Further application of the multi-laboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784). CONCLUSION: The inter-laboratory reproducibility determined for this method met the acceptance criteria defined in AOAC SMPR 2018.010. HIGHLIGHTS: AOAC has approved the method for Final Action Status.

Modeling of Integrated Hollow-Fiber Solar-Powered VMD Modules for Desalination for a Better Understanding and Management of Heat Flows.

The direct integration of membrane distillation and solar energy collection in a single module is a promising technology for autonomous seawater desalination in remote regions; however, the modeling and design of such modules are challenging because of the coupling of the radial and longitudinal heat and mass transfers. In a previous study, we provided as a first modeling approach a hollow fiber solar collector vacuum membrane distillation (VMD) module, considering a constant temperature at the shell side and a pure water feed. Here, a full model is developed to describe the coupled effects of the solar collector and a hollow fiber VMD module operating in an outside/in mode with saline water. The model considers all the main phenomena (membrane distillation, temperature and concentration polarization, absorption of solar radiation and energy balances over the solar collector, radial and longitudinal heat and mass transfer, seawater properties, and more than 30 variables). Applied to simulate the behavior of a semi-industrial-scale module, it allows the influence of solar radiation on the performance/limits of the integrated module to be discussed based on the radial and longitudinal profiles and heat flows. The model can be used to identify key points in the module design to better utilize solar radiation and manage heat flows.

Confirmation of the full conversion of ethylene oxide to 2-chloroethanol in fumigated foodstuffs: possible implications for risk assessment.

This study describes the extension of a gas chromatography mass spectrometry (GC-MS) method, initially devoted to the analysis of ethylene oxide (EO) in ice cream, to a larger range of food items including herbs, spices, vegetables, inorganic salts, food supplements, thickeners, etc. Results are reported as EOTotal according to EC 2015/868 definition (expressed as EO equivalents as the sum of native EO and 2-chloroethanol (2-CE) after acidic hydrolysis) with a limit of quantification at 0.01 mg/kg regardless of the food item. Its ruggedness was demonstrated through fortification experiments on hundreds of samples. Re-analysis of 146 positive food samples without hydrolysis demonstrated that not EO but 2-CE is the predominant analyte detected in the different processed ingredients suspected to have been previously treated with EO. A series of eight contaminated dried herbs and spices were also re-analysed by four ISO 17025 accredited commercial laboratories making use of different analytical strategies for EO determination in foods. Each laboratory reported EOTotal levels within the same concentration range, but the resulting reproducibility ranged from 23% to 41% depending on the sample. Additionally, we show that results of free EO from methods based on conversion to 2-iodoethanol may lead to artefactual detection of native EO (false positive). An official method of analysis applicable for different food matrices would be useful to avoid discrepancies of results. Altogether, these data re-enforce the fact that in absence of native EO in food items, risk assessment of EO in foodstuffs should consider the predominance of 2-CE. A toxicological risk assessment using the food additive xanthan gum as a case study is discussed.

Traces of 2-phenylphenol in roasted coffee are not related to agrochemical residue in green coffee beans, but to generation during roasting.

Traces of the phytosanitary agent 2-phenylphenol in roasted coffee are not necessarily related to residues of agrochemicals. This study shows that roasting of coffee generates 2-phenylphenol at low level. Green coffee samples (approx. 1500) were found negative for 2-phenylphenol and the levels of 2-phenylphenol increased as a function of roasting degree. Packaging materials as a source of contamination can be excluded. The exposure to 2-phenylphenol by coffee consumption is negligible and contributes to less than 0.004% of the ADI. The presence of 2-phenylphenol residues in roasted coffee above the regulatory limits for green coffee must not necessarily lead to the conclusion that the green coffee, either conventional or organic, was non-compliant.

A new analytical protocol for the determination of 62 endocrine-disrupting compounds in indoor air.

The objective of this study was to develop and validate a new analytical protocol for simultaneous determination of 62 semi-volatile organic compounds in both phases of indoor air. Studied compounds belong to several families: polybrominated diphenyl ethers, polychlorinated biphenyls, hexachlorobenzene, pentachlorobenzene, phthalates, polyaromatic hydrocarbons, parabens, tetrabromobisphenol A, bisphenol A, hexabromocyclododecane, triclosan, alkylphenols, alkylphenol ethoxylates, synthetic musks (galaxolide and tonalide) and pesticides (lindane and cypermethrin). A medium volume sampling system was used to collect simultaneously these endocrine-disrupting compounds (EDCs) from the gaseous and particulate phases. An accelerated solvent extraction method was optimized to obtain all EDCs in a single extract by atmospheric phase. Their extraction from the sorbents and their analysis by liquid and gas chromatography-mass spectrometry (LC/MS/MS, GC/MS and GC/MS/MS) was validated using spiked sorbents (recovery study and analytical uncertainty analysis by fully nested design). The developed protocol achieved low limits of quantification (<0.5ng m(-3)) and low uncertainty values (<5ng m(-3)) for all compounds. Once validated, the method was applied to indoor air samples from four locations (a house, an apartment, a day nursery and an office) and compared to literature to confirm its efficiency. All target EDCs were quantified in the samples and were primarily present in the gaseous phase. The major contaminants found in indoor air were, in descending order, phthalates, synthetic musks, alkylphenols and parabens.

Adsorption combined with ultrafiltration to remove organic matter from seawater.

Organic fouling and biofouling are the major severe types of fouling of reverse osmosis (RO) membranes in seawater (SW) desalination. Low pressure membrane filtration such as ultrafiltration (UF) has been developed as a pre-treatment before reverse osmosis. However, UF alone may not be an effective enough pre-treatment because of the existence of low-molecular weight dissolved organic matter in seawater. Therefore, the objective of the present work is to study a hybrid process, powdered activated carbon (PAC) adsorption/UF, with real seawater and to evaluate its performance in terms of organic matter removal and membrane fouling. The effect of different PAC types and concentrations is evaluated. Stream-activated wood-based PAC addition increased marine organic matter removal by up to 70% in some conditions. Moreover, coupling PAC adsorption with UF decreased UF membrane fouling and the fouling occurring during short-term UF was totally reversible. It can be concluded that the hybrid PAC adsorption/UF process performed in crossflow filtration mode is a relevant pre-treatment process before RO desalination, allowing organic matter removal of 75% and showing no flux decline for short-term experiments.

Vacuum membrane distillation of seawater reverse osmosis brines.

Seawater desalination by Reverse Osmosis (RO) is an interesting solution for drinking water production. However, because of limitation by the osmotic pressure, a high recovery factor is not attainable. Consequently, large volumes of brines are discharged into the sea and the flow rate produced (permeate) is limited. In this paper, Vacuum Membrane Distillation (VMD) is considered as a complementary process to RO to further concentrate RO brines and increase the global recovery of the process. VMD is an evaporative technology that uses a membrane to support the liquid-vapour interface and enhance the contact area between liquid and vapour in comparison with conventional distillation. This study focuses on VMD for the treatment of RO brines. Simulations were performed to optimise the operating conditions and were completed by bench-scale experiments using actual RO brines and synthetic solutions up to a salt concentration of 300 g L(-1). Operating conditions such as a highly permeable membrane, high feed temperature, low permeate pressure and a turbulent fluid regime allowed high permeate fluxes to be obtained even for a very high salt concentration (300 g L(-1)). For the membrane studied, temperature and concentration polarisation were shown to have little effect on permeate flux. After 6 to 8 h, no organic fouling or biofouling was observed for RO brines. At high salt concentrations, scaling occurred (mainly due to calcium precipitation) but had only a limited impact on the permeate flux (24% decrease for a permeate specific volume of 43L m(-2) for the highest concentration of salt). Calcium carbonate and calcium sulphate precipitated first due to their low solubility and formed mixed crystal deposits on the membrane surface. These phenomena only occurred on the membrane surface and did not totally cover the pores. The crystals were easily removed simply by washing the membrane with water. A global recovery factor of 89% can be obtained by coupling RO and VMD.