Preparative isolation of (+)-beta-eudesmol fromAmyris balsamifera

Summary Optically pure (+)-beta-eudesmol is a possible starting material for the synthesis of several termite defense compounds. A two step procedure for the isolation of gram quantities of (+)-beta-eudesmol from commercially availableAmyris balsamifera oil (syn. West Indian sandalwood oil), containing 8% beta-eudesmol, was developed. Step one consisted of an efficient vacuum distillation of the total oil. Step two was a medium pressure LC separation with an AgNO₃ impregnated silica gel stationary phase. Several other separation procedures failed due to the presence of many closely related sesquiterpene alcohols (75% of the oil).     

Electrochemical detection of nitrate,nitrite and ammonium for on-site water quality monitoring

This review examines the most recent electrochemical developments for nitrate, nitrite and ammonium detection for on-site water monitoring. There remains a high demand for effective field-based detection of the dissolved inorganic nitrogen (DIN) analytes to aid in mitigating nitrogen loading. Electrochemical approaches show increasing potential to fill this role as advancements in nanotechnology continually improve analytical performance and on-site applicability. However, translating these improvements into the field still faces the resonating challenges of reaching analytical proficiency (selectivity, sensitivity, robustness, stability), practical end-user functionality, minimal matrix interferences and cost effectiveness. Herein, we elaborate on these challenges via a critical evaluation of current studies and examine how realistic the prospects of on-site nitrate, nitrite and ammonium are. We also present recommendations in addressing these gaps to conclude the review.     

Out-of-plane deflections of metallic and composite pin-loaded coupons

The projection shadow moiré technique was employed to determine an out-of-plane contouring history of aluminum, [(+45/–45)]_3S , [(0/90₃,0] _S and [(0/90/+45/–45)]_2S fiberglass epoxy pin-loaded specimens experimentally. The contouring interval was limited to 0.0254 mm by experimental concerns. Qualification of the projection shadow moiré optical arrangement was initially accomplished by the out-of-plane contouring of a clamped, centrally loaded, circular aluminum plate. Experimental results indicate significant out-of-plane displacements in the bearing region of the coupon at load levels well below ultimate. Effects of material anisotropy could be seen in the fiber-oriented shape of the displacement contours. Comparisons with three-dimensional finite-element results indicate that experimental out-of-plane contours were significantly larger than their finite-element counterparts in the region above the pin for the [(+45/–45)]_3S , [(0/90)₃, 0] _S laminates. These deviations increased with increasing pin-load level. These variations could be attributed to linear-elastic through-thickness moduli assumptions as well as through-thickness finite-element mesh coarseness.     

Über die Anwendung elektrometrischer Methoden zur Bestimmung pharmazeutischer Produkte. VII

Zusammenfassung Es werden einige Methoden zur Bestimmung des Hydrazids der Iso-Nicotinsäure beschrieben. Folgende Reaktionen werden hierfür verwendet: Die Oxydation des Hydrazinrestes, die Überführung des Hydrazids in das Azid sowie die Bestimmung der sauren und basischen Gruppen durch Titration in nichtwäßriger Lösung.Der Endpunkt der jeweiligen Reaktion wird entweder mit Indikatoren, besser und genauer aber elektrometrisch bestimmt.

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Summary Several methods for the determination of the hydrazide of iso-nicotinic acid are described. The following reactions were used for this purpose: oxidation of the hydrazine radical; conversion of the hydrazide to the azide; determination of the acidic and basic groups by titration in non-aqueous solution. The endpoint of the particular titration is determined either by means of indicators, or better and more accurately electrometrically.

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Résumé On décrit quelques méthodes pour le dosage de l'hydrazide de l'acide isonicotinique. Les réactions suivantes ont été utilisées pour cela: l'oxydation du reste hydrazide, la transformation de l'hydrazide en azide ainsi que le dosage des groupements acides et basiques par titrage en milieu non aqueux. Le point d'équivalence est déterminé suivant le cas soit avec des indicateurs, soit mieux et d'une façon plus précise électrométriquement.

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Mit 4 Abbildungen.     

Über das polarographische Verhalten des Iso-Nicotinsäurehydrazids

Zusammenfassung Es wird eine Methode der polarographischen Bestimmung des Hydrazids der Iso-Nicotinsäure beschrieben. Es werden Angaben über die Feststellung von dessen Zersetzungsprodukten in pharmazeutischen Zubereitungen gemacht.

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Summary A method for the polarographic determination of the hydrazide of isonicotinic acid is described. Statements are made concerning the establishment of its decomposition products in pharmaceutical preparations.

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Résumé On décrit une méthode de dosage polarographique de l'hydrazide de l'acide iso-nicotinique. On donne des indications pour rechercher des produits de décomposition de celui-ci dans des préparations pharmaceutiques.

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Mit 7 Abbildungen.     

Rate constants for: OH + NO2 (+ N2) → HNO3 (+ N2) between 220 and 358 K

Rate constants have been determined for the reaction OH + NO₂ (+ N₂) → HNO₃ (+ N₂), using time-resolved resonance absorption to follow the removal of OH radicals produced by flash photolysis of HNO₃. The measurements cover the ranges: 220 ? T ? 358 K and 3.2 × 10¹⁷ ? [N₂] ? 4.0 × 10¹⁸ molecule cm^?3.     

Longitudinal Bottom-Up Proteomics of Serum,Serum Extracellular Vesicles,and Cerebrospinal Fluid Reveals Candidate Biomarkers for Early Detection of Glioblastoma in a Murine Model

Glioblastoma Multiforme (GBM) is a brain tumor with a poor prognosis and low survival rates. GBM is diagnosed at an advanced stage, so little information is available on the early stage of the disease and few improvements have been made for earlier diagnosis. Longitudinal murine models are a promising platform for biomarker discovery as they allow access to the early stages of the disease. Nevertheless, their use in proteomics has been limited owing to the low sample amount that can be collected at each longitudinal time point. Here we used optimized microproteomics workflows to investigate longitudinal changes in the protein profile of serum, serum small extracellular vesicles (sEVs), and cerebrospinal fluid (CSF) in a GBM murine model. Baseline, pre-symptomatic, and symptomatic tumor stages were determined using non-invasive motor tests. Forty-four proteins displayed significant differences in signal intensities during GBM progression. Dysregulated proteins are involved in cell motility, cell growth, and angiogenesis. Most of the dysregulated proteins already exhibited a difference from baseline at the pre-symptomatic stage of the disease, suggesting that early effects of GBM might be detectable before symptom onset.     

Orotic acid: a milk constituent Enzymatic determination by means of a new microcalorimetric method

The presence of orotic acid (a precursor of nucleic acid) in milk is very important in order to ensure its nutritional value and good conservation. In the literature, chromatographic, spectrophotometric and polarographic methods are reviewed. The reported values have a very wide interval range (19-664 mg l(-1)) and a low precision. The new method proposed in this article employs an enzymatic reaction. It has been improved on standards and then tested on milk samples. The same samples were also tested by means of a known spectrophotometric method. The new analytical method for orotic acid determination is reliable; the results are more accurate and more precise if compared with the usual methods, and it shows the same sensibility. The calorimetric analysis is faster and easier, owing to the fact that no sample treatments are required.