Optimisation of mild-acidic protein extraction from defatted sunflower (Helianthus annuus L.) meal

For protein isolation from defatted sunflower meal, mild-acidic extraction was investigated to minimise concomitant oxidation and polymerisation of phenolic compounds and their irreversible binding to proteins. Because of the impaired solubility of sunflower proteins at low pH, the potential of sodium chloride (NaCl) to improve protein extractability was firstly screened for pH 2–11. Increasing NaCl concentrations of the aqueous solvent (c_NaCl) up to 2.8 mol/L enhanced the relative protein yield to almost 80% at ambient temperature and pH 5.6–7.4. As to improved protein recovery at minimal interactions with phenolic acids, the concerted effects of pH (3.2–7.4), c_NaCl (1–3 mol/L), temperature (T, 15–45 °C), and meal-to-solvent ratio (MSR, 0.03 and 0.05 g/mL) on the protein concentration of the extract (c_PE) and the relative protein yield (RPY) were examined, using response surface methodology (RSM). Aside from the prevailing influence of pH value and salt concentration, elevated temperature slightly enhanced protein extraction, whereas MSR mainly influenced c_PE, but hardly RPY. Calculated models proved suitable for the evaluation of extraction processes and the prediction of optimum conditions in terms of high protein yields at the lowest pH possible. Extraction at pH 6.0 was shown to be an appropriate compromise yielding 76–83% of the meal protein, depending on the constraints given. With elevated NaCl concentrations compensating for unfavourable pH conditions, mild-acidic extraction was found to be suitable for the recovery of high-quality sunflower protein in terms of light-coloured protein isolates.     

Improving Interoperability by Incorporating UnitsML Into Markup Languages

Maintaining the integrity of analytical data over time is a challenge. Years ago, data were recorded on paper that was pasted directly into a laboratory notebook. The digital age has made maintaining the integrity of data harder. Nowadays, digitized analytical data are often separated from information about how the sample was collected and prepared for analysis and how the data were acquired. The data are stored on digital media, while the related information about the data may be written in a paper notebook or stored separately in other digital files. Sometimes the connection between this “scientific meta-data” and the analytical data is lost, rendering the spectrum or chromatogram useless. We have been working with ASTM Subcommittee E13.15 on Analytical Data to create the Analytical Information Markup Language or AnIML—a new way to interchange and store spectroscopy and chromatography data based on XML (Extensible Markup Language). XML is a language for describing what data are by enclosing them in computer-useable tags. Recording the units associated with the analytical data and metadata is an essential issue for any data representation scheme that must be addressed by all domain-specific markup languages. As scientific markup languages proliferate, it is very desirable to have a single scheme for handling units to facilitate moving information between different data domains.At NIST, we have been developing a general markup language just for units that we call UnitsML. This presentation will describe how UnitsML is used and how it is being incorporated into AnIML.     

Herausforderungen an Füge‐ und Oberflächentechnik für zukünftige Leichtbaukonstruktionen im Automobilbau

For the reduction of the weight of vehicle hot‐rolled magnesium alloys as well as carbon fiber reinforced plastics (CFK) shall be integrated into the body structure. Both light weight materials electrochemically are not compatible with galvanized steels or aluminium alloys, unless great efforts of corrosion protection measures are taken. From electrochemical investigations an oxidceramic surface layer deposited by plasmachemical oxidation can be recommended as a promising solution. The low‐porous oxidation deposit with limited insulation effect can be painted by e‐coat in high quality after joining in the body shop and before the full paint system will be deposited. In opposite to magnesium CFK parts have, however, electrochemically a very noble character causing galvanic corrosion of attached metallic parts when the carbon fibers are not fully embedded in the matrix or damaged by the cutting. Only joining elements made from stainless steels or titanium alloys (e. g. Ti‐6Al‐4V) are suitable for the joining of CFK by screwdriving and riveting technology to avoid galvanic corrosion. From view of compatibility of materials, a severe anodic corrosion risk can be eliminated by isolation through adhesive bonding in the flanges and an additional sealing to prevent from electrolyte ingress.     

Sila-haloperidol, a silicon analogue of the dopamine (D2) receptor antagonist haloperidol: synthesis, pharmacological properties, and metabolic fate

Haloperidol (1 a), a dopamine (D(2)) receptor antagonist, is in clinical use as an antipsychotic agent. Carbon/silicon exchange (sila-substitution) at the 4-position of the piperidine ring of 1 a (R(3)COH --> R(3)SiOH) leads to sila-haloperidol (1 b). Sila-haloperidol was synthesized in a new multistep synthesis, starting from tetramethoxysilane and taking advantage of the properties of the 2,4,6-trimethoxyphenyl unit as a unique protecting group for silicon. The pharmacological profiles of the C/Si analogues 1 a and 1 b were studied in competitive receptor binding assays at D(1)-D(5), sigma(1), and sigma(2) receptors. Sila-haloperidol (1 b) exhibits significantly different receptor subtype selectivities from haloperidol (1 a) at both receptor families. The C/Si analogues 1 a and 1 b were also studied for 1) their physicochemical properties (log D, pK(a), solubility in HBSS buffer (pH 7.4)), 2) their permeability in a human Caco-2 model, 3) their pharmacokinetic profiles in human and rat liver microsomes, and 4) their inhibition of the five major cytochrome P450 isoforms. In addition, the major in vitro metabolites of sila-haloperidol (1 b) in human liver microsomes were identified using mass-spectrometric techniques. Due to the special chemical properties of silicon, the metabolic fates of the C/Si analogues 1 a and 1 b are totally different.     

High-affinity, selective σ ligands of the 1,2,3,4-tetrahydro-1,4'-silaspiro[naphthalene-1,4'-piperidine] type: syntheses, structures, and pharmacological properties

The 1'-organyl-1,2,3,4-tetrahydrospiro[naphthalene-1,4'-piperidine] derivatives 1?a-4?a [for which organyl=benzyl (1?a), 4-methoxybenzyl (2?a), 2-phenylethyl (3?a), or 3-methylbut-2-enyl (4?a)] are high-affinity, selective σ? ligands. The corresponding sila-analogues 1?b-4?b (replacement of the carbon spirocenter with a silicon atom) were synthesized in multistep syntheses, starting from dichlorodivinylsilane, and were isolated as the hydrochlorides 1?b?HCl-4?b?HCl. Compounds 1?a?HCl-4?a?HCl and 1?b?HCl-4?b?HCl were structurally characterized by NMR spectroscopy (1H, 13C, 2?Si) in solution, and the C/Si analogues 3?a?HCl and 3?b?HCl were studied by single-crystal X-ray diffraction. These structural investigations were complemented by computational studies. The σ? and σ? receptor affinities of the C/Si pairs 1?a/1?b-4?a/4?b were studied with radioligand binding assays. The σ? receptor affinity of the silicon compounds 1?b-4?b is slightly higher than that of the corresponding carbon analogues 1?a-4?a. Because affinity for the σ? receptor is decreased by the C/Si exchange, the σ?/σ? selectivity of the silicon compounds is considerably improved, indicating that the C→Si switch strategy is a powerful tool for modulating both pharmacological potency and selectivity.     

Comparison of fatty acid profiles and contents of seed oils recovered from dessert and cider apples and further Rosaceous plants

To get a more comprehensive knowledge of oil contents and fatty acid pattern, seed oils from various Rosaceous plants belonging to the subfamilies Maloideae and Rosoideae, respectively, were investigated. For this purpose, isolated seeds of 18 dessert and cider apple (Malus domestica BORKH.) cultivars of different provenances, pear (Pyrus communis L.), rose hip (Rosa canina L.), quince (Cydonia oblonga Mill.), and red chokeberry (Aronia arbutifolia L.) were analyzed for their oil content and fatty acid composition. Oil contents varied significantly, not only among the different genera, but also among cultivars of one species, ranging from 0.8 to 29.4?g/100?g?dry matter. Qualitatively, the fatty acid profiles of the investigated seed oils showed good agreement in all representatives of the Rosaceae. Their triacylglycerols were uniformly composed of linoleic, oleic, palmitic, stearic, palmitoleic, α-linolenic, arachidic, gondoic, and behenic acids. Quantitation of individual fatty acids revealed the oils to be rich in mono- and diunsaturated oleic acid and linoleic acid, ranging from 15.1 to 33.3?g/100?g and from 32.5 to 49.7?g/100?g, respectively. As expected, contents of saturated fatty acids were 6–10?times lower. Moreover, apple cultivars showed pronounced differences in yields, numbers, and weights of their seeds. As demonstrated by the data obtained from this study, seeds resulting from the processing of apple, pear, quince, chokeberry (Maloideae), and rose hip (Rosoideae) into juices, jellies, and jams may serve as a promising source for the recovery of nutritionally valuable edible oils.     

Thermal inactivation of strawberry polyphenoloxidase and its impact on anthocyanin and color retention in strawberry (Fragaria x ananassa Duch.) purées

Strawberry (Fragaria x ananassa Duch.) cultivars were screened for their polyphenoloxidase (PPO) activities, and thermal stability of PPO was evaluated in vitro for three cultivars under different time–temperature regimes (60, 75 and 90 °C for 3 and 5 min, respectively). Heating strawberry purées should further elucidate the impact of thermal treatments on strawberry PPO in its natural matrix (‘in situ’ activity). To evaluate the consequences of PPO inactivation on anthocyanin and color stability, the purées were stored for 28 days at +20 °C monitoring the contents of monomeric, polymeric (spectrophotometrically) and individual anthocyanins (HPLC–DAD–MSⁿ) as well as color properties (CIE L*a*b*). Antioxidant activities (FRAP), total phenolic (Folin–Ciocalteu) and ascorbic acid contents of freshly prepared and stored purées, respectively, were determined spectrophotometrically. PPO activities varied considerably among the cultivars investigated. Accordingly, different time–temperature regimes were required for their complete in vitro and in situ inactivation. Unexpectedly, thermal inactivation of PPO was disadvantageous regarding pigment and color retention of strawberry purées, which was ascribed to partial regeneration of PPO. Hence, protection of antioxidants, total phenolics and ascorbic acid from oxidative degradation could not be achieved by heating the purées prior to storage.