Non-targeted screening for contaminants in paper and board food-contact materials using effect-directed analysis and accurate mass spectrometry

Due to large knowledge gaps in chemical composition and toxicological data for substances involved, paper and board food-contact materials (P&B FCM) have been emerging as a FCM type of particular concern for consumer safety. This study describes the development of a step-by-step strategy, including extraction, high-performance liquid chromatography (HPLC) fractionation, tentative identification of relevant substances and in vitro testing of selected tentatively identified substances. As a case study, we used two fractions from a recycled pizza box sample which exhibited aryl hydrocarbon receptor (AhR) activity. These fractions were analysed by gas chromatography (GC) and ultra-HPLC (UHPLC) coupled to quadrupole time-of-flight mass spectrometers (QTOF MS) in order tentatively to identify substances. The elemental composition was determined for peaks above a threshold, and compared with entries in a commercial mass spectral library for GC-MS (GC-EI-QTOF MS) analysis and an in-house built library of accurate masses for substances known to be used in P&B packaging for UHPLC-QTOF analysis. Of 75 tentatively identified substances, 15 were initially selected for further testing in vitro; however, only seven were commercially available and subsequently tested in vitro and quantified. Of these seven, the identities of three pigments found in printing inks were confirmed by UHPLC tandem mass spectrometry (QqQ MS/MS). Two pigments had entries in the database, meaning that a material relevant accurate mass database can provide a fast tentative identification. Pure standards of the seven tentatively identified substances were tested in vitro but could not explain a significant proportion of the AhR-response in the extract. Targeted analyses of dioxins and PCBs, both well-known AhR agonists, was performed. However, the dioxins could explain approximately 3% of the activity observed in the pizza box extract indicating that some very AhR active substance(s) still remain to be identified in recycled low quality P&B.     

Identification of benzalkonium chloride in food additives and its inefficacy against bacteria in minced meat and raw sausage batters

There is a growing market for 'natural' food preservatives though their active ingredients are poorly known. We analysed four such additives, Bacterin, Protecta One, Protecta Two and Protecta Three, marketed as effective preservatives for meat products on the basis of salts and extracts of 'natural herbs'. Their ingredients were separated by HPLC and the structures of the antimicrobially active components were determined by mass spectrometry. The products contained the disinfectant benzalkonium chloride, an antimicrobial quaternary ammonium compound, as the only active principle. HPLC methods are reported for the analysis of benzalkonium chloride in such products and in meat. Bacterin and Protecta One, as well as pure benzalkonium chloride in equivalent concentrations, did not show antibacterial effects against meat-relevant pathogens in minced meat and raw sausage batter. Because benzalkonium chloride is not a permitted food additive, and is not effective as a preservative in meat, the public should be cautioned against such products alleged to contain 'natural herb extracts'.     

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Inactivation of staphylococcal enterotoxins by heat and reactivation by high pH treatment

Inactivation of staphylococcal enterotoxins (SE) added to different media upon heat treatment (80 degrees C or 100 degrees C for 10 min) and reactivation of inactivated SE was studied. In gelatin (pH 4.0), lettuce extract, peas and beans extracts and ovalbumin (pH 5.0) the immunological activity of SE was lost almost completely upon heating. The loss of immunological activity of SEA was accompanied by a concomitant loss of biological activity of this toxin (monkey feeding test). A high pH treatment (pH 11) of the different preparations restored both the immunological and biological activity in most samples tested. Heating at 80 degrees C or 100 degrees C for 10 min of SE containing gelatin (pH 7.0), cauliflower extract (pH 4.0 or pH 7.0), milk (pH 4.0), casein (pH 6.0), rice extract (pH 7.0), noodles extract (pH 4.0) and oat-flakes extract (pH 7.0) had a much lower effect on the immunological activity of the SE (activity greater than or equal to 25%).     

Characterization of Cementitious Materials Exposed to Freezing and Thawing in Combination with Deicing Salts Using 3D Scans

Surface deterioration of concrete subjected to freezing and thawing in combination with deicing salts is one of the most important factors determining the durability of concrete infrastructure in cold climates. The freeze–thaw deicing salt (FTDS) resistance of cementitious materials can be determined by the capillary suction of de-icing chemicals and freeze–thaw (CDF) test. Specimens are subjected to repeated freeze–thaw cycles with simultaneous addition of deicing salt and the amount of material scaled off near the surface is determined. For concretes with adequate FTDS resistance, this test method works very well. However, specimens with unknown performance often experience increased edge scaling. This leads to a falsification of results and consequently to an underestimation of the actual freeze–thaw resistance. In materials research, however, concretes with high levels of surface deterioration are studied in order to investigate various factors of influence on the freeze–thaw resistance of concretes in a targeted manner. This article presents a novel methodology that delivers new information regarding surface deterioration of CDF samples using high-resolution 3D scan data. Change of volume is used to support deterioration results of the standard CDF methodology. Increase of surface area is used to estimate change in roughness of samples.     

Gate leakage current reduction in IP3 SRAM cells at 45 nm CMOS technology for multimedia applications

We have presented an analysis of the gate leakage current of the IP3 static random access memory (SRAM) cell structure when the cell is in idle mode (performs no data read/write operations) and active mode (performs data read/write operations), along with the requirements for the overall standby leakage power, active write and read powers. A comparison has been drawn with existing SRAM cell structures, the conventional 6T, PP, P4 and P3 cells. At the supply voltage, V_DD = 0.8 V, a reduction of 98%, 99%, 92% and 94% is observed in the gate leakage current in comparison with the 6T, PP, P4 and P3 SRAM cells, respectively, while at V_DD = 0.7 V, it is 97%, 98%, 87% and 84%. A significant reduction is also observed in the overall standby leakage power by 56%, the active write power by 44% and the active read power by 99%, compared with the conventional 6T SRAM cell at V_DD = 0.8 V, with no loss in cell stability and performance with a small area penalty. The simulation environment used for this work is 45 nm deep sub-micron complementary metal oxide semiconductor (CMOS) technology, t_ox = 2.4 nm, V_thn = 0.22 V, V_thp = 0.224 V, V_DD = 0.7 V and 0.8 V, at T = 300 K.     

Increasing the effective interfacial area in plastic packed absorption columns.

Effective interfacial areas for gas absorption were measured at various irrigation rates for Raschig rings made of a ceramic (industrial porcelain) and of various plastics. The plastics used were polyethylene and polypropylene having very low wettabilities with water. The surface of some of the plastic packings was covered with a hydrophilic layer. The absorption of pure oxygen by a sodium sulphite solution containing cobalt catalyst was used for the measurement of effective interfacial area. It has been found that the effective interfacial area of plastic packings was about 40 per cent of that of geometrically similar ceramic packings. The effective interfacial area of the plastic packings was increased about 2·5 times by application of the hydrophilic layer. Thus, the wetted surface areas of plastic packings with hydrophilic surface and of ceramic packings are practically the same.     

Negative electrodes for nickel-cadmium accumulators: their properties as determined by impregnation procedure

Sintered negative electrodes for nickel-cadmium secondary cells were studied. Model electrodes prepared by means of three different impregnation methods were evaluated. It was demonstrated that the impregnation procedure may affect properties of active mass and the service life of electrodes in a significant way.