Development of a bioanalytical method for the quantification of sinococuline in human plasma and its application in phase I clinical pharmacokinetic study

A selective, highly sensitive, precise, and novel bioanalytical method has been developed and validated to quantify sinococuline, an active constituent present in the phytopharmaceutical drug product containing Cocculus hirsutus plant extract, in vivo. Chromatographic separation was achieved on a Luna Omega Polar-C18 bonded analytical column maintained at 45°C. The isocratic mobile phase consisted of methanol and ammonium formate buffer (60:40, v/v) at acidic pH with a low flow rate of 0.250 mL/min. Detection was performed on an API 4000 mass spectrometer using electrospray ionization in positive polarity and multiple reaction monitoring mode to achieve a lower limit of quantification of 1.50 ng/mL. Excellent accuracy and precision were obtained after extracting the analyte from plasma samples using a chemical analogue as an internal standard in the absence of an isotope-labeled compound. The extraction efficacy was evidenced from recovery study, and the analyte was found to be stable in plasma. Validation study demonstrated linearity with coefficient of correlation, r ≥ 0.99, and minimal matrix effect. This bioanalytical method was successfully applied to evaluate pharmacokinetic parameters of sinococuline from a phase I clinical trial of an aqueous extract of C. hirsutus in healthy human volunteers.     

Micro-mechanical behaviors of SMA composite materials under hygro-thermo-elastic strain fields

An analytical procedure to evaluate the behavior of shape memory alloy (SMA) composite under hygrothermal environment is presented. The SMA wires are considered as inclusions embedded in a homogeneous matrix medium of the composite. The inhomogeneity associated with the phase transformation and thermal strains in the SMA wire as well as the hygrothermal strain in the matrix is homogenized using Eshelby’s equivalent inclusion method. In the present work, a similar approach adopted for SMA composites by Marfia and Sacco [Marfia, S., Sacco, E., 2005. Micromechanics and homogenisation of SMA-wire-reinforced materials. J. Appl. Mech. 72 (2), 259–268.] is considered in order to validate the response of SMA composite subjected to thermo-elastic strain field. However, in the present approach, certain modifications and new derivations for the inelastic strain tensors is carried out. First, the constitutive laws for the SMA wire and matrix are expressed in terms of the average strain in the composite. The evolutionary equations used to characterize the pseudoelastic (PE) behavior of the SMA wire are redefined in terms of the eigen strains (phase transformation and thermal strains) occurring in the SMA wire, which are then expressed in terms of the average strain in the composite. Further, the SMA composite constitutive law under coupled hygro-thermo-elastic strain fields is proposed. The generic homogenized hygric and thermal inelastic composite tensors required for the proposed hygro-thermo-elastic constitutive law are derived. Finally, the SMA composite lamina is characterized using Eshelby’s equivalent inclusion method. Using the proposed modifications and derivations, the analytical results are validated for the case of thermo-elastic strain fields and the procedure is then extended to evaluate the SMA composite behavior under hygro-thermo-elastic strain fields. The results include the effect of thermo-elastic and hygro-thermo-elastic strains on the transformation stresses and the nature of hysteresis due to hygric and thermo-elastic strains.     

Untersuchung der OberflÄchenspannung der Systeme:

Zusammenfassung Die Oberfl?chenspannungen der Systeme: 1. Wasser/propionsaures Natrium mit verschiedenen Alkoholen; 2. Wasser/buttersaures Natrium mit verschiedenen Alkoholen; 3. Wasser/crotonsaures Natrium mit verschiedenen Alkoholen und 4. Wasser/caprylsaures Natrium mit verschiedenen Alkoholen wurden gemessen, und die Ergebnisse werden im Sinne der in früheren Arbeiten (3, 4) ver?ffentlichten Hypothese diskutiert.

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Summary The surface tension of the systems (1) water-sodium propionate and different alcohols, (2) water-sodium butyrate and different alcohols, (3) water-sodium crotonate and different alcohols and (4) water-sodium caprylate and different alcohols has been determined and the results have been discussed on the basis of the hypothesis suggested in previous papers (3, 4).

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übersetzt von Dr. K, Jaeckel (Marburg/L.)

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Wir danken Herrn Dr. A. Chatterji, Head of the Chemistry Department, für sein Entgegenkommen. Einer von uns (J. M.) dankt dem Scientific Research Grants Committee für ein Stipendium zur Durchführung der Arbeit.     

Schiff base complexes of dioxouranium(VI). VII. Dioxouranium(VI) acetate complexes with monobasic bidentate and bibasic tridentateSchiff bases

11 and 12 molar reactions of dioxouranium(VI) acetate dihydrate with the monobasic bidentateSchiff bases,o-HOC₆H₄CH=NR oro-HOC₁₀H₆CH=NR (R=C₂H₅,n-C₃H₇,n-C₄H₉ or C₆H₅) and bibasic tridentateSchiff bases,o-HOC₆H₄CH=NR(OH) oro-HOC₁₀H₆CH=NR(OH) (R=–CH₂CH(CH₃)- or —CH₂CH₂CH₂–) have been studied and derivates of the type UO₂(OAc)₂(SBH), UO₂(OAc)₂(SBH)₂, UO₂(OAc)₂(SBH ₂) and UO₂(OAc)₂(SBH ₂)₂ (whereSBH andSBH ₂ represent monobasic bidentate and bibasic tridentateSchiff base molecules respectively) have been isolated. These have been characterized by elemental analysis, conductance measurements and IR spectral studies.

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UO₂ ²⁺-Komplexe von Schiff-Basen. VII. Uranylacetat-Komplexe mit monobasischen zweizähnigen und bibasischen dreizähnigen Schiff-Basen

Zusammenfassung Es wurden in 1:1- und 1:2-molaren Reaktionen von UO₂(OAc)₂·2H₂O mitSchiff-Basen (L) Komplexe des Typs UO₂(OAc)₂ L bzw. UO₂(OAc)₂ L ₂ isoliert. Die Komplexe wurden mittels Elementaranalyse, Leitfähigkeitsmessungen und IR-Spektren untersucht.

     

Mischligandenderivate des 1:1-Th(IV)—DTPA-Chelates mit Milchs?ure, Mandels?ure und o-Hydroxynaphthoes?uren

Potentiometric studies of the mixed ligand derivatives of 11-Th(IV)—DTPA chelate (whereDTPA=diethylene-triamine pentaacetic acid) with certain secondary ligands, such as lactic, mandelic and o-hydroxynaphthoic acids have been carried out. The pH-titrations of the reaction mixtures containing 111 molar ratio of metal ion toDTPA to secondary ligand have shown the formation of 111 ternary complexes at higher pH (8). The equilibrium constants of the resulting mixed complexes have been determined at 30±1°C and =0.1 (KNO₃) and the order of stability in terms of secondary ligands has been found to be o-hydroxy naphthoic acids>mandelic acid>lactic acid.     

Synthesis and structural studies of complexes of Sb(III) and Bi(III) with thiosemicarbazones

Summary Several new complexes of Sb(III) and Bi(III) with thiosemicarbazones of furfuraldehyde, thiophene-2-carbaldehyde, indol-3-carbaldehyde and pyridine-2-carbaldehyde have been prepared and characterized by elemental analysis, conductivity, molecular weight determination and IR,¹H-and¹³C-NMR spectral studies. The ligands form complexes of the typeMX ₃ L[M=Sb(III) or Bi(III);X=chloride;L=ligand] which are found to be non-electrolytes inDMF. Spectral data indicate that the thiosemicarbazones act as bidentate ligands through the azomethine nitrogen and sulphur.

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Synthese und Strukturuntersuchungen an Komplexen von Sb(III) and Bi(III) mit Thiosemicarbazonen

Zusammenfassung Es wurden einige neue Komplexe von Sb(III) und Bi(III) mit Tiosemicarbazonen von Furfural, Thiophen-2-carbaldehyd, Indol-3-carbaldehyd und Pyridin-2-carbaldehyd hergestellt und mittels Elementaranalyse, Leitfähigkeitsmessungen, Molekulargewichtsbestimmungen und IR-,¹H- bzw.¹³C-NMR-Spektroskopie charakterisiert. Die Komplexe sind vom TypMX ₃ L[M=Sb(III) oder Bi(III);X=Chlorid;L=Ligand] und sind inDMF Nichtelektrolyten. Die spektroskopischen Daten zeigen, daß die Thiosemicarbazone als zweizähnige Liganden über den Azomethin-Stickstoff und Schwefel wirken.

     

Thermal and biological studies of Schiff bases of chitosan derived from heteroaryl aldehydes

Journal of Thermal Analysis and Calorimetry - The synthesis of Schiff bases of chitosan is performed by the reaction of chitosan with different heteroaryl aldehydes, i.e., furfuraldehyde,...