Concurrent determination of olanzapine,risperidone and 9‐hydroxyrisperidone in human plasma by ultra performance liquid chromatography with diode array detection method: application to pharmacokinetic study

A simple and sensitive ultra‐performance liquid chromatography (UPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ), risperidone (RIS) and 9‐hydroxyrisperidone (9‐OHRIS) in human plasma in vitro. The sample preparation was performed by simple liquid–liquid extraction technique. The analytes were chromatographed on a Waters Acquity H class UPLC system using isocratic mobile phase conditions at a flow rate of 0.3 mL/min and Acquity UPLC BEH shield RP₁₈ column maintained at 40°C. Quantification was performed on a photodiode array detector set at 277 nm and clozapine was used as internal standard (IS). OLZ, RIS, 9‐OHRIS and IS retention times were found to be 0.9, 1.4, .1.8 and 3.1 min, respectively, and the total run time was 4 min. The method was validated for selectivity, specificity, recovery, linearity, accuracy, precision and sample stability. The calibration curve was linear over the concentration range 1–100 ng/mL for OLZ, RIS and 9‐OHRIS. Intra‐ and inter‐day precisions for OLZ, RIS and 9‐OHRIS were found to be good with the coefficient of variation <6.96%, and the accuracy ranging from 97.55 to 105.41%, in human plasma. The validated UPLC method was successfully applied to the pharmacokinetic study of RIS and 9‐OHRIS in human plasma. Copyright © 2015 John Wiley & Sons, Ltd.     

A novel fast method for aqueous derivatization of THC,OH‐THC and THC‐COOH in human whole blood and urine samples for routine forensic analyses

A novel aqueous in situ derivatization procedure with propyl chloroformate (PCF) for the simultaneous, quantitative analysis of Δ⁹‐tetrahydrocannabinol (THC), 11‐hydroxy‐Δ⁹‐tetrahydrocannabinol (OH‐THC) and 11‐nor‐Δ⁹‐tetrahydrocannabinol‐carboxylic acid (THC‐COOH) in human blood and urine is proposed. Unlike current methods based on the silylating agent [N,O‐bis(trimethylsilyl)trifluoroacetamide] added in an anhydrous environment, this new proposed method allows the addition of the derivatizing agent (propyl chloroformate, PCF) directly to the deproteinized blood and recovery of the derivatives by liquid–liquid extraction. This novel method can be also used for hydrolyzed urine samples. It is faster than the traditional method involving a derivatization with trimethyloxonium tetrafluoroborate. The analytes are separated, detected and quantified by gas chromatography–mass spectrometry in selected ion monitoring mode (SIM). The method was validated in terms of selectivity, capacity of identification, limits of detection (LOD) and quantification (LOQ), carryover, linearity, intra‐assay precision, inter‐assay precision and accuracy. The LOD and LOQ in hydrolyzed urine were 0.5 and 1.3 ng/mL for THC and 1.2 and 2.6 ng/mL for THC‐COOH, respectively. In blood, the LOD and LOQ were 0.2 and 0.5 ng/mL for THC, 0.2 and 0.6 ng/mL for OH‐THC, and 0.9 and 2.4 ng/mL for THC‐COOH, respectively. This method was applied to 35 urine samples and 50 blood samples resulting to be equivalent to the previously used ones with the advantage of a simpler method and faster sample processing time. We believe that this method will be a more convenient option for the routine analysis of cannabinoids in toxicological and forensic laboratories.     

The pharmacokinetics and tissue distribution of curcumin and its metabolites in mice

Curcumin (CUR) is the major active component of turmeric and plays an important role in the prevention and treatment of many chronic diseases such as respiratory and neurodegenerative disease. In the present work, a rapid and simple LC–MS/MS method was developed to investigate the pharmacokinetics and tissue distribution of CUR and its metabolites in mice after intravenous administration of CUR (20 mg/kg). The results showed that the values of AUC_0–∞ were 107.0 ± 18.3, 6.0 ± 1.2 and 12.0 ± 4.0 (mg/L) min, and those for t_1/2z were 32.4 ± 10.8, 6.4 ± 2.4 and 5.6 ± 1.8 min for CUR, dihydrocurcumin (DHC) and tetrahydrocurcumin (THC) in plasma, respectively. CUR and THC could be detected in liver while CUR and DHC were detected in kidney. Only CUR was detected in brain. These findings indicated that THC was the main metabolite of CUR in plasma. The exposure of CUR in plasma was 6‐fold greater than that in liver, kidney and brain.     

Synthesis,characterization and biological screening studies of mixed ligand complexes using flavonoids as precursors

Flavonoids are a group of plant phenolics that provide various health benefits through cell signalling pathways and antioxidant effects. In the present study, a new series of mixed ligand complexes of Co(II), Ni(II), Cu(II) and Zn(II) were synthesized by incorporating curcumin and quercetin flavonoid precursors. The structural features of the synthesized complexes were explored using elemental analysis, thermogravimetric analysis, UV–visible, infrared, NMR, mass and electron paramagnetic resonance spectral analyses and conductivity measurements. These data support an octahedral geometry of the synthesized complexes. In silico biological activity score for the ligand was predicted using PASS online software. ADMET properties were studied using VLS3D online software. Anti‐inflammatory and antioxidant activities were experimentally validated which prove that theoretical predictions are in agreement with the experimental results. Interestingly the synthesized complexes interact with calf thymus DNA through groove binding mode. Moreover, they have good potential to cleave pUC19 DNA. Minimum inhibitory concentration values of the synthesized complexes reveal that they have better antimicrobial efficacy than the ligands.     

Colloidal Synthesis and Photophysics of M3Sb2I9 (M=Cs and Rb) Nanocrystals: Lead‐Free Perovskites

Herein we report the colloidal synthesis of Cs₃Sb₂I₉ and Rb₃Sb₂I₉ perovskite nanocrystals, and explore their potential for optoelectronic applications. Different morphologies, such as nanoplatelets and nanorods of Cs₃Sb₂I₉, and spherical Rb₃Sb₂I₉ nanocrystals were prepared. All these samples show band‐edge emissions in the yellow–red region. Exciton many‐body interactions studied by femtosecond transient absorption spectroscopy of Cs₃Sb₂I₉ nanorods reveals characteristic second‐derivative‐type spectral features, suggesting red‐shifted excitons by as much as 79 meV. A high absorption cross‐section of ca. 10⁻¹⁵ cm² was estimated. The results suggest that colloidal Cs₃Sb₂I₉ and Rb₃Sb₂I₉ nanocrystals are potential candidates for optical and optoelectronic applications in the visible region, though a better control of defect chemistry is required for efficient applications.     

Some Useful Integral Representations for Information-Theoretic Analyses

This work is an extension of our earlier article, where a well-known integral representation of the logarithmic function was explored and was accompanied with demonstrations of its usefulness in obtaining compact, easily-calculable, exact formulas for quantities that involve expectations of the logarithm of a positive random variable. Here, in the same spirit, we derive an exact integral representation (in one or two dimensions) of the moment of a nonnegative random variable, or the sum of such independent random variables, where the moment order is a general positive non-integer real (also known as fractional moments). The proposed formula is applied to a variety of examples with an information-theoretic motivation, and it is shown how it facilitates their numerical evaluations. In particular, when applied to the calculation of a moment of the sum of a large number, n, of nonnegative random variables, it is clear that integration over one or two dimensions, as suggested by our proposed integral representation, is significantly easier than the alternative of integrating over n dimensions, as needed in the direct calculation of the desired moment.     

Metal–organic framework of amine‐MIL‐53(Al) as active and reusable liquid‐phase reaction inductor for multicomponent condensation of Ugi‐type reactions

Metal–organic framework of NH₂‐MIL‐53(Al), with coordinative unsaturated aluminium sites, has been shown to be active in the Groebke–Blackburn–Bienaymé multicomponent coupling reaction based on Ugi‐type amine and aldehyde condensation over isocyanide and then a cyclization process. Interestingly this reaction occurred under solvent‐free conditions with high yield, in which the NH₂‐MIL‐53(Al) could be recovered and reused for five reaction cycles, giving a total turnover number of 455.     

Studies of phase transitions and ferroelastic domain walls in Pb5Al3F19 crystals by optical measurements

Three phase transitions between 100 and 400 K were previously shown by X-ray diffraction measurements. Such results have been confirmed by optical measurements on crystals. The thermal dependence of the birefringence has been determined. A new phase transformation has been shown at around 590 K not only by optical study but also by dielectric measurements. Ferroelastic domain-walls have been visualized. The sequence transition has been discussed taking into account the various space groups.     

Cross section of the impact single ionization of B2＋ by H＋

The ionization process of B2+ by H+ impact is studied using the continuum-distorted-wave eikonal-initial-state (CDW-EIS) method and the modified free electron peak approximation (M-FEPA), respectively. Total, single-, and double- differential cross sections from 1s and 2s orbitals are presented for the energy range from 10 keV/u to 10 MeV/u. Comparison between the results from the two methods demonstrates that the total and single-differential cross sections for the high-energy incident projectile case can be well evaluated using the simple M-FEPA model. Moreover, the M-FEPA model reproduces the essential features of the binary-encounter (BE) bump in the double-differential cross sections. Thus, the BE ionization mechanism is discussed in detail by adopting the M-FEPA model. In particular, the double- and single-differential cross sections from the 2s orbital show a high-energy hip, which is different from those from the 1s orbital. Based on Ref. [1], the Compton profiles of B2+ for 1s and 2s orbitals are given, and the hips in DDCS and SDCS from the 2s orbital are explained.     

Analytic approximation of the blow‐up time for nonlinear differential equations by the ADM–Padé technique

We present a new approach to calculate analytic approximations of blow‐up solutions and their critical blow‐up times. Our approach applies the Adomian decomposition–Padé method to quickly and easily compute the critical blow‐up times, which comprises the Adomian decomposition method combined with the Padé approximants technique. We validate our new approach with a variety of numerical examples, including nonlinear ODEs, systems of nonlinear ODEs, and nonlinear PDEs. Furthermore, our new method is shown to be more convenient than prior art that relies on compound discretized algorithms. Copyright © 2013 John Wiley & Sons, Ltd.