Stir bar sorptive extraction of diclofenac from liquid formulations: A proof of concept study

A new stir bar sorptive extraction (SBSE) technique coupled with HPLC-UV method for quantification of diclofenac in pharmaceutical formulations has been developed and validated as a proof of concept study. Commercially available polydimethylsiloxane stir bars (Twister (TM)) were used for method development and SBSE extraction (pH, phase ratio, stirring speed, temperature, ionic strength and time) and liquid desorption (solvents, desorption method, stirring time etc) procedures were optimised. The method was validated as per ICH guidelines and was successfully applied for the estimation of diclofenac from three liquid formulations viz. Voltarol (R) Optha single dose eye drops, Voltarol (R) Ophtha multidose eye drops and Voltarol (R) ampoules. The developed method was found to be linear (r=0.9999) over 100-2000 ng/ml concentration range with acceptable accuracy and precision (tested over three QC concentrations). The SBSE extraction recovery of the diclofenac was found to be 70% and the LOD and LOQ of the validated method were found to be 16.06 and 48.68 ng/ml, respectively. Furthermore, a forced degradation study of a diclofenac formulation leading to the formation of structurally similar cyclic impurity (indolinone) was carried out. The developed extraction method showed comparable results to that of the reference method, i.e. method was capable of selectively extracting the indolinone and diclofenac from the liquid matrix. Data on inter and intra stir bar accuracy and precision further confirmed robustness of the method, supporting the multiple re-use of the stir bars. (C) 2010 Elsevier B.V. All rights reserved.

Determination of diclofenac from paediatric urine samples by stir bar sorptive extraction (SBSE)-HPLC-UV technique

A novel stir bar sorptive extraction (SBSE) method coupled with high performance liquid chromatography (HPLC) and UV detection for the extraction of diclofenac (DIC) from paediatric urine samples has been developed and validated. Selectivity and sensitivity being the prime objectives of the bioanalytical method for clinical samples, an optimised SBSE protocol was developed that selectively extracted DIC from various concurrently administered drugs. The validated assay was found to be linear (r=0.9999) over a concentration range of 100-2000 ng mL(-1). SBSE showed consistent recoveries (similar to 70%) of DIC across the validated linearity range. Overall, the method exhibited excellent accuracy and precision across all QC concentrations, tested over three days. Calculated LOD and LOQ were found to be 12.03 ng mL(-1) and 36.37 ng mL(-1), respectively, however, for the experimental purposes, 100 ngmL(-1) was considered as the validated LOQ(accuracy and precision at this LQC was

Using bar-code technology to capture clinical intervention data in a hospital with a stand-alone pharmacy computer system

The use of barcode technology to capture data on pharmacists' clinical interventions is described.

An ESPRIT-SAA-Based Detection Method for Broken Rotor Bar Fault in Induction Motors

This paper presents a novel detection method for broken rotor bar fault (BRB) in induction motors based on Estimation of Signal Parameters via Rotational Invariance Technique (ESPRIT) and Simulated Annealing Algorithm (SAA). The performance of ESPRIT is tested with simulated stator current signal of an induction motor with BRB. It shows that even with a short-time measurement data, the technique is capable of correctly identifying the frequencies of the BRB characteristic components but with a low accuracy on the amplitudes and initial phases of those components. SAA is then used to determine their amplitudes and initial phases and shows satisfactory results. Finally, experiments on a 3kW, 380V, 50Hz induction motor are conducted to demonstrate the effectiveness of the ESPRIT-SAA-based method in detecting BRB with short-time measurement data. It proves that the proposed method is a promising choice for BRB detection in induction motors operating with small slip and fluctuant load.

FRENKEL-KONTOROVA DOMAIN-WALL PHASE-TRANSITIONS IN AN ADSORBED LAYER - POTASSIUM ON CO(10(1)OVER-BAR-0)

As the potassium fractional coverage of a cobalt {1010BAR} surface is increased over the range 0.2 to 0.6 monolayer the adlayer passes through a series of phase transitions. A commensurate phase is formed at exactly 0.5 monolayer, and corresponds to adatoms bonded in high-symmetry hollow sites on the unreconstructed cobalt surface, with an effective adatom radius lying between the ionic and covalent radii of potassium. A detailed structural study shows that the structural transitions can be characterised within a one-dimensional Frenkel-Kontorova model, with small lateral displacements of adatoms away from hollow sites in the low and high coverage phases. The low coverage phases progress from a distributed vacancy structure to a low density domain-wall structure; while the high coverage phase formed above half a monolayer is a high density asymmetric domain-wall structure.

Analytical model for bar-end cover separation failure in RC beams strengthened with near-surface mounted FRP

The flexural performance of RC beams can be improved using the near-surface mounted (NSM) FRP strengthening technique. A likely failure mode of such FRP-strengthened RC beams is bar-end cover separation which involves the detachment of the NSM FRP reinforcement together with the concrete cover along the level of the steel tension reinforcement. This paper presents a new analytical strength model for this failure mode. The proposed strength model and two existing strength models for this failure mode are compared with test results to demonstrate the superior performance of the new analytical model.