A simple procedure for the chromatographic isolation and determination of prostaglandins from human seminal plasma

Summary A relatively simple procedure for the isolation and determination of the prostaglandins present in human seminal fluid is described. It involves preliminary chromatographic purification of these compounds from the major non-prostaglandin impurities followed by their total elution in one solvent (one-step elution). The prostaglandins thus obtained were almost free from other lipids and were further resolved into prostaglandin-groups and individual prostaglandins by repeated thin-layer chromatography. Data are also presented for prostaglandin contents of fresh semen samples from five individuals and results compared with those from the stored samples.

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Einfaches Verfahren zur chromatographischen Isolierung und Bestimmung von Prostaglandinen aus menschlichem Sperma

Zusammenfassung Das Verfahren umfaßt eine chromatographische Abtrennung der Verbindungen von den hauptsächlichsten Verunreinigungen und die Gesamtelution mit einem Lösungsmittel. Die von anderen Lipiden fast völlig freien Prostaglandine werden durch wiederholte Dünnschicht-Chromatographie in Gruppen und Einzelverbindungen getrennt. Werte werden angegeben über die Prostaglandingehalte von frischem im Vergleich zu gelagertem Sperma.

     

Role of partially flocculated sols in emulsion stability

Summary The stability of emulsion of Toluene in water stabilized by partially flocculated ferric hydroxide sol has been studied. The size of the emulsion droplets as determined by size frequency analysis is found to be of 1.1 μ radius. The flocculation studies were carried out haemocytometrically at different amount of electrolytes and at different p_H values. The electrokinetic potential ‘ζ’ was determined micro-electrophoretically at different amounts of electrolytes and also at different p_H's. In the case of tri and tetra valent anions the charge reversal was observed. In the light of the D.V.O. theory the interaction energy profiles were drawn and 2–6 kT deep secondary minima obtained showing thereby the occurrence of reversible flocculation. Degree of aggregation has been calculated theoretically at different values of ‘A’ and the value of A was found to be 1.0×10⁻¹² erg to fit the value of degree of aggregation obtained haemocytometrically. The charge densities and binding parameters have also been calculated.     

Thiotropolone as a chromogenic reagent for the simultaneous determination of cobalt(II) and nickel(II)

Thiotropolone forms chloroform-soluble reddish-brown and violet complexes with cobalt(II) and nickel(II), in the pH range 7.0-8.5 and 6.0-9.0 respectively. Based on this, a sensitive and rapid method for the spectrophotometric determination of traces of cobalt and nickel in metals and alloys has been developed. The two metals can be determined accurately in the range 0.6-2.6 ppm of cobalt and 0.75-4.57 ppm of nickel, simultaneously.     

Force constants,coriolis coupling constants and mean amplitudes of vibration of GaF63− and FeF63−

The force constants, Coriolis coupling constants and mean amplitudes of vibration at 0, 298.16 and 500 K for GaF₆^3?FeF₆^3? have been reported for the first time employing recent vibrational data. The results are discussed in the light of available information.     

Intensities of wagging and rocking bands of water in MnCl2 · 2H2O and CoCl2 · 2H2O

IR relative integrated intensities and half-widths of rocking (R) and wagging (W) bands of water in MnCl₂ · 2H₂O and CoCl₂ · 2H₂O are presented at 300 K and 120 K. Departure of observed intensity into D_W/D_R from those predicted by the fixed dipole model is attributed to anisotropic dynamic changes in dipole during these oscillations. A quantity representing the variation of this anisotropy between W and R oscillations is computed and its origin is discussed. An increase by 20% to 50% in both D_W and D_R on lowering the temperature has also been discussed.     

An iodine-123 generator/iodination kit: A preliminary report

Preliminary results are described of a¹²³Xe filled device to serve as a combination¹²³I generator/iodination kit.¹²³X was produced in the Brookhaven Linac Isotope Producer (BLIP) by the reaction¹²⁷I(p, 5n)¹²³Xe. The device consists of a small glass ampoule containing an internal glass breakseal and a flanged neck on which was crimped a multi-injection type septum. The ampoule contained a hydrogen sulfide atmosphere to assure that the iodine generated from the decay of the xenon was in the form of iodide. Following an adequate period for¹²³Xe to decay (this period can be used for shipment), a needle is forced through the septum breaking the seal and residual gases are pumped off. The¹²³I in the form of iodide can then be rinsed from the ampoule with any desired solvent or reagent added directly to the device to carry out an iodination in an enclosed environment. Preliminary results of both iodine recovery and iodinations have been promising. This research was supported by the US Department of Energy under Contract No. DE-ACO2-76CH0016.     

On the estimation of higher order resistance coefficients from electroosmotic transport data

Summary First and second order resistance coefficients between membrane matrix and permeant for the permeation of methanol, acetone and methyl ethyl ketone through pyrex and quartz membranes have been evaluated from the experimental data on electroosmotic effects. Analysis of the data shows that-the following non-linear relationP =R ₁₁ J _v +R ₁₂ I +R ₁₂₂ I ²[1] exists between pressure difference,P, and the fluxes and a linear relation =R ₂₁ J _v +R ₂₂ I [2] expresses the dependence of potential difference,, on the fluxes. The first order cross resistance coefficients have been found to obey theOnsager's reciprocity relation. An attempt has been made to explain the occurrence of higher order resistance coefficients in terms of electrokinetic character of the membrane, permeant interface.

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Zusammenfassung Die Widerstandskoeffizienten 1. und 2. Ordnung zwischen einer Membranmatrix und dem permeierenden Stoff wurden für die Permeation von Methanol, Aceton und Methyläthylketon durch Pyrex- und Quarz-Membranen auf Grund elektroosmotischer Effekte bestimmt. Die Auswertung gibt die nichtlineare BeziehungP =R ₁₁ J _v +R ₁₂ I +R ₁₂₂ I ² [1] zwischen der Druckdifferenz und dem Fließen; die lineare Beziehung =R ₂₁ J _v +R ₂₂ I [2] beschreibt die Abhängigkeit der Potentialdifferenz vom Fließen. Die gekreuzten Widerstandskoeffizienten 1. Ordnung gehorchen dem ReziprozitätsgesetzOnsager. Das Vorkommen von Widerstandskoeffizienten höherer Ordnung wird versuchsweise auf den elektrokinetischen Charakter der Membran-Grenzfläche zurückgeführt.

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With 2 figures and 2 tables     

Spectrophotometric Determination of Palladium with Methylthymol Blue

A new, sensitive spectrophotometric method for the determination of palladium(II) with methylthymol blue has been developed. The palladium methylthymol blue complex has an absorption maximum at 530 nm. The colour reaction has a sensitivity of 0.005 µg of palladium/cm² and obeys Beer's Law over the range 0.4 to 3.24 ppm of palladium. The effects of concentration of perchloric acid, reagent, heating, stability of colour and diverse ions have been investigated. The ratio of metal: ligand in the complex is 1:1 and the formation constant was calculated to be 1.18×10⁴.     

Stability of AQUO-organic silver iodide sol

Summary The coagulation concentration for silver iodide sol, both in presence of pyridine and dioxane, increases for mono- and bivalent coagulating electrolyte. In presence of a mixture of pyridine and dioxane in equal volume, the coagulation concentration assumes an intermediate value, which is nearer to dioxane. However, in presence of dioxane more bivalent electrolyte is needed than in presence of pyridine. If a bivalent coagulating electrolyte is added to a sol containing a mixture of pyridine and dioxane, the amount of electrolyte required to coagulate is less than pyridine and greater than dioxane. Thus silver iodide sol is more stable toward mono- and bivalent coagulating electrolytes. The degree of stabilization increases with the decrease of the dielectric constant of the dispersing medium. The intermediate values for dioxane pyridine mixture is accountable by the fact that dioxane acts as a solvent for pyridine. The PH value of the sol increases up to the coagulation point. Beyond this, there is an abrupt decrease. When the particles settle down completely a rise in PH is again noted on the further addition of electrolytes. The increase in the electrical conductance is more significant after coagulation. These changes have been explained by adsorption of the ions and due to the release of ions from the electrical double layer.

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Zusammenfassung Die Koagulationskonzentration für Silberjodidsol in Gegenwart von Pyridin und Dioxan steigt für ein- und zweiwertige Elektrolyte an. In Gegenwart einer Mischung zu gleichen Volumen erh?lt man mittlere Werte, n?her denen zu Dioxan. Für Koagulation in Gegenwart von Dioxan ist jedoch mehr zweiwertiger Elektrolyt notwendig als in Gegenwart von Pyridin. Bei Koagulation mit zweiwertigem Elektrolyt verbraucht ein Sol mit der Mischung von Pyridin und Dioxan weniger als für Pyridin und mehr als für Dioxan. Daher ist das Silbersol gegenüber ein- und zweiwertigen Elektrolyten stabiler. Der Grad der Stabilisierung w?chst mit abnehmender Dielektrizit?tskonstante des Dispersionsmediums. Die Zwischenwerte der Dioxan-Pyridin-Mischungen lassen sich verstehen durch die Tatsache, da? Dioxan als L?sungsmittel für Pyridin wirkt. Der PH-Wert des Sols w?chst bis zum Koagulationspunkt, darüberhinaus erfolgt ein steiler Abfall. Wenn die Teilchen vollst?ndig absetzen, ist bei weiterer Zugabe von Elektrolyt ein erneuter Anstieg im PH feststellbar. Der Anstieg der elektrolytischen Leitf?higkeit wird nach der Koagulation ausgepr?gter. Diese ?nderungen lassen sich durch Ionenadsorption und Freiwerden von Ionen aus der elektrischen Doppelschicht erkl?ren.

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Our thanks are due to Prof. R. C. Mehrotra for providing all the facilities for this work and to Prof. S. Ghosh of Allahabad University for helpful discussions. Thanks are also due to the University Grants Commission, Government of India, for the award of a research scholarship to one of us (V. K. S.).