Method for Control of Particle Size and Morphology of Paraffin/Polystyrene-Divinylbenzene Microcapsules

Microencapsulation of phase change materials(Micro PCMs) has been paid special attention because of their extensive applications in saving and releasing energy. Micro PCMs containing paraffin with a melting point of 55 ℃ in polystyrene-divinylbenzene(P(St-DVB)) were prepared by suspension-like polymerization. The characterization of microcapsules by FTIR, DSC and TG proved that paraffin had been successfully encapsulated and the proportion of encapsulated paraffin was 49.8%—58.5%. The effects of polyvinylpyrrolidone(PVP) with different molecular weights serving as the suspension stabilizer were investigated in detail. The results illustrated that the type of PVP had a significant influence on the particle size of Micro PCMs. The average diameter of Micro PCMs decreased with an increasing molecular weight of PVP. Moreover, the crosslinker-postaddition method was adopted in this study to improve the morphology of P(St-DVB) Micro PCMs. SEM images showed that when the DVB was added at the 2nd hour of polymerization the morphology of obtained P(St-DVB) Micro PCMs exhibited good sphericity since it could avoid the influence of cross-linker agent during the nucleation period.

Determination of Aroclor 1254 in Water Samples Using Polystyrene-Divinylbenzene Solid-Phase Extraction and Gas Chromatography

A method was developed for the determination of Aroclor 1254 in water samples using polystyrene-divinylbenzene(PS-DVB)solid-phase extraction(SPE)and gas chromatography(GC).The PS-DVB sorbent demonstrated good recoveries of Aroclor 1254 when sulfuric acid(1:1,v:v)was added to the samples.Sample quantification was performed using gas chroma-tography with a parallel column and dual electron capture detector.Factors in extraction method procedures were optimized,including sample pH,elution solvent,eluting volume and breakthrough volume.With the 1000 ml sample acidified to pH 1.0,a 6.0 ml n-hexane/ethyl acetate(1:1,v:v)elution solvent,and gas chromatographic determination,the recoveries of Aroclor 1254 in spiked water samples ranged from 90.6 to 104%.Across testing days,repeatability ranged from 4.7 to 7.6%.The method detection limit was 0.053μg/L.PS-DVB exhibited a broader pH stability range,satisfactory recoveries,and good repeatability for Aroclor 1254 extraction.The results indicate that these methods can be used to analyze trace amounts of Aroclor 1254,and represent a new analytical approach for determining polychlorinated biphenyls in water samples.

A Comparative Evaluation of Polystyrene Divinylbenzene Copolymer HPLC Columns on the Chromatographic Performance of the Compendial Method for Doxycycline Hyclate Capsules: Implications for Method Implementation of a Medical Countermeasure Medication

The purpose of this study was to evaluate the impact of polystyrene divinylbenzene copolymer HPLC columns on the chromatographic performance of the USP compendial method for doxycycline hyclate. The compendial method was implemented based on the assessment of the chromatographic performance of six USP defined L21 polystyrene divinylbenzene HPLC columns. Modifications to the method were based on USP for chromatography. The method was validated for the determination of doxycycline hyclate and its impurities in commercially available drug products. A number of different polystyrene-divinylbenzene columns were tested and failed to provide selectivity for the resolution of doxycycline and its impurities. Separation was optimally achieved on an Agilent PLPR-S column (250 × 4.6 mm, 8 μm) by using an Agilent 1260 series HPLC system. Doxycycline hyclate and its impurities were eluted isocratically at a flow rate of 1 mL/min with mobile phase and detected at 270 nm. The column temperature was maintained at 60oC. The method was validated according to USP category I requirements for Assay. Validation acceptance criteria were met in all cases. The analytical range for doxycycline hyclate was 50 - 250 μg/mL and the linearity was r2 > 0.999 over three days. The method was determined to be specific. Both accuracy (95.1% - 102.4%) and precision (0.50% - 4.8%) were established across the analytical range for low, intermediate and high QC concentrations. Method applicability was demonstrated by analyzing marketed products of doxycycline hyclate, in which results showed potency meeting USP acceptance criteria. In conclusion, this study described the remarkable differences in selectivity that were encountered during the implementation phase for the compendial methods for doxycycline and its impurities in marketed products and it could be used in the future to assss the product quality of doxycycline hyclate capsules stored in the National stockpiles.