The effect of phosphate buffer solutions on uniconazole complexation with hydroxypropyl-β-cyclodextrin and methyl-β-cyclodextrin

The inclusion complexes of uniconazole [(E)-1-(4-chlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-lyl)-1-penten-3-ol, UCZ] with two cyclodextrin derivatives, hydroxypropyl-β-cyclodextrin (HP-β-CD) and methylated-β-cyclodextrin (Me-β-CD), were prepared and characterized by ¹H NMR and FT-IR. The phase solubility of UCZ and HP-β-CD, UCZ and Me-β-CD, which displays the ability of CDs complexation and solubilization, was studied in aqueous solutions and phosphate buffer solutions (PBS) with different property pH values (6.2, 7.2, 8.0). The solubility results indicated that the pH of PBS showed more enhancement on the interaction of HP-β-CD and UCZ than Me-β-CD with the increasing pH value, and the optimal pH value for complexation of UCZ and HP-β-CD, UCZ and Me-β-CD was at 8.0 and at 7.2, respectively. These were also determined by UCZ release behavior and dissolution studies of the complexes in solid state.     

Fabrication of a sol–gel derived microporous zirconia membrane for nanofiltration

This paper reports the fabrication and nanofiltration properties of a sol–gel derived microporous zirconia membrane. Effects of synthesis parameters, including hydrolysis time, hydrolysis temperature, hydrolysis ratio and chelating agent dopant, on the state and size of polymeric zirconia sol, were investigated. Highly reproducible and stable zirconia sol after refluxing at 40 °C for 180 min, with an average particle size of approximately 8.6 nm, was synthesized with a recipe of [Zirconium n-propoxide]: [Diethanolamine]: [1-propanol]: [H₂O] being 1: 2.2: 28.7: 9.4 (in molar ratio). The sol was subsequently used for the fabrication of microporous ZrO₂ membranes onto alumina supported mesoporous γ-Al₂O₃ layers. ZrO₂ membranes with molecular weight cut-off (MWCO) of 354, 1,195, corresponding to the pore size of 0.94 and 1.75 nm, were successfully fabricated. Ionic retention properties of such ZrO₂ membranes with respect to electrolyte solutions, like MgCl₂, CaCl₂, NaCl and Na₂SO₄, were also determined. Effects of parameters such as concentration of salt solutions and trans-membrane pressure on retention rates of microporous ZrO₂ membranes were studied in detail. Results showed that zirconium n-propoxide derived microporous ZrO₂ membranes exhibited comparatively high retention rates towards divalent ions like Mg²⁺ and Ca²⁺, while much lower retention rates were observed for mono-valent ion (Na⁺) in the present study, which are the characteristics of nanofiltration membranes.     

Tuner design and RF test of a four-rod RFQ

A mini-vane four-rod radio frequency quadruple (RFQ) accelerator has been built for neutron imaging. The RFQ will operate at 201.5 MHz, and its length is 2.7 m. The original electric field distribution along the electrodes is not flat. The resonant frequency needs to be tuned to the operating value. And the frequency needs to be compensated for temperature change during high power RF test and beam test. As tuning such a RFQ is difficult, plate tuners and stick tuners are designed. This paper will present the tuners design, the tuning procedure, and the RF properties of the RFQ.

     

Development and validation of UPLC‐MS/MS method for determination of domperidone in human plasma and its pharmacokinetic application

A sensitive, rapid and selective ultra‐performance liquid chromatography–tandem mass spectrometric (UPLC‐MS/MS) method was developed for the determination and pharmacokinetic study of domperidone in human plasma. Diphenhydramine was used as the internal standard. Plasma sample pretreatment involved a one‐step liquid–liquid extraction with a mixture of diethyl ether–dichloromethane (3:2, v/v). The analysis was carried out on an Acquity UPLC^TM BEH C₁₈ column. The mobile phase consisted of methanol–water containing 10 mmol/L ammonium acetate and 0.5% (v/v) formic acid (60:40, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionizationsource with positive mode. Each plasma sample was chromatographed within 2.1 min. The standard curves for domperidone were linear (r² ≥ 0.99) over the concentration range of 0.030–31.5 ng/mL with a lower limit of quantification of 0.030 ng/mL. The intra‐ and inter‐day precision (relative standard deviation) values were not higher than 13% and accuracy (relative error) was from ?7.6 to 1.2% at three quality control levels. The method herein described was superior to previous methods and was successfully applied to the pharmacokinetic study of domperidone in healthy Chinese volunteers after oral administration. Copyright © 2012 John Wiley & Sons, Ltd.     

Evaluation of approximations for concentration-dependent micropore diffusion in sorbent with bidisperse pore structure

Average diffusivity linear driving force (AD-LDF) and concentration-dependent diffusivity linear driving force (CDD-LDF) approximations are introduced to simplify the precise model describing the concentration-dependent micropore diffusion in bidisperse sorbents, and are compared with the precise model in predicting the dynamics of a sorption process under two different perturbations (i.e., step change perturbations and sinusoidal wave perturbation) with different concentrations imposed at the exterior surface of the bidisperse sorbent. The performance of the two approximations is validated by the precise model and experiments. The AD-LDF performs better in step adsorption and CDD-LDF does better in step desorption. Under sinusoidal wave perturbation, the CDD-LDF performs better. The different levels of consistency of the two approximations with the precise model are attributed to the different definitions of the diffusivities.