Improvement of Nanoprecipitation Technique for Preparation of Gelatin Nanoparticles and Potential Macromolecular Drug Loading

An optimum nanoprecipitation technique for gelatin nanoparticles is established, based on aqueous gelatin solution and ethanolic solution containing stabilizer. Crosslinking with glutaraldehyde results in stable gelatine nanoparticles. Several factors such as the surfactant concentration, type of surfactant, type of nonsolvent and gelatin concentration are evaluated. Gelatin nanoparticles with 200–300 nm can be produced using 20–30 mg mL^?1 of gelatin and a minimum of 7% w/v stabilizer (Poloxamer 407 or 188). Furthermore, methanol and ethanol are good nonsolvents, whereas other nonsolvents such as acetone, isopropyl alcohol, and acetonitrile, result in phase separation and visible precipitates. The entrapment efficiency of fluorescein‐isothiocyanate (FITC)‐dextran as model drug was determined to 50% with no substantial effect on particle size. 80% of the drug is only released after enzymatic digestion.

     

A Simple and Convenient One-Pot Synthesis of Benzimidazole Derivatives Using Cobalt(II) Chloride Hexahydrate as Catalyst

A simple and efficient method for the convenient synthesis of 2-arylbenzimidazole has been described on reaction with o-phenylenediamine and various aromatic aldehydes using cobalt(II) chloride hexahydrate as a catalyst. The method is cost-effective, high-yielding, clean, and selective.     

Synthesis of Trichlorophenol Derivatives

An expedient three‐step procedure for the synthesis of trichlorophenol derivatives based on the acid‐catalyzed rearrangement of the bicyclic ketone precursors 6a–e in high overall yield is described. The bicyclic ketone precursors 6a–e were obtained from Diels–Alder cycloadducts of β‐substituted vinyl acetates with tetrachloro‐5,5‐dimethoxycyclopentadiene in two steps.     

Simple and Convenient Synthesis of 21‐Thioalkylether Derivatives of Methyl 16‐Prednisolone Carboxylates

The antedrug approach for corticosteroids has been described as a fundamentally sound approach for the development of safer anti‐inflammatory and anti‐asthmatic therapy. However, the derivatization of prednisolone and its congeners have been considered to be major pitfalls, because their syntheses are complicated by the presence of numerous carboxylate esters and hydroxyl functions in the steroid nucleus. A simple and direct synthesis of 21‐thioalkylether derivatives of methyl 16‐prednisolonecarboxylates is described. The 21‐mesylate of the methyl 16‐prednisolonecarboxylate and 9‐fluoro‐17‐dehydro methyl 16‐prednisolonecarboxylate were reacted with Na‐thioalkoxides to furnish the desired thioethers in good yields. A previously published method for the methanolysis of 16‐cyanoprednisolone to methylcarboxylate has been reexamined, and the conditions are explained clearly. The reaction conditions for all these reactions were critical.     

Measurement of natural radioactivity in soil from Peshawar basin of Pakistan

Natural radioactivity in the environment may change with time due to human activities, chemical and biological changes. From the view of radiation risk to population, the knowledge of natural radioactivity levels and the measurement of collective radiation dose received by the population is very vital. Radiological constraints on soil of thickly populated Peshawar basin in northern Pakistan were assessed through radiometric assay. Soil samples collected from different locations of four districts of this basin were analysed using an HPGe gamma spectrometer. Activity concentrations of ⁴⁰K, ²²⁶Ra and ²³²Th in these samples was 648 ± 121 (421–996), 45 ± 7 (32–60) and 59 ± 7 (46–72) Bq kg^?1, respectively that followed lognormal distribution. The average concentrations of primordial radionuclides were found to be higher than that reported for the worldwide soil. Radium equivalent activity and gamma index derived from these activity concentrations were lesser than their respective limits. The average absorbed dose rate and the annual effective dose for both indoor and outdoor cases were found to be higher than the values given in the UNSCEAR 2000 report. The results of the present study were compared with those for other locations of Pakistan along with that for the world. The radiological impact of the measured data was evaluated using hazard assessment models. A thoughtful discussion of the above mentioned evaluation is also given.     

Determination of phosphate in freshwater samples by flow-injection with lucigenin chemiluminescence

Lucigenin chemiluminescence (CL) in conjunction with flow-injection analysis (FIA) is used for the determination of phosphate in freshwater samples. The procedure is based on the formation of molybdophosphoric heteropoly acid (MoP–HPA) by the reaction of phosphate and ammonium molybdate under acidic conditions. CL emission was observed as a result of oxidation of lucigenin in aqueous sodium hydroxide solution in the presence of MoP–HPA. Calibration was linear up to 500?µg?L^?1 (r ^2?=?0.9998; n?=?8), with a detection limit (S/N?=?3) of 0.95?µg?L^?1. An injection throughput of 120 h^?1, and relative standard deviation (RSD; n?=?4) of 1.3–3.2% were achieved in the concentration range studied. An on-line chelating column was used to remove interfering cations. The method was applied to freshwater samples, and the results (51?±?1.0 – 107?±?2.0?µg?L^?1) did not differ significantly from results obtained using a spectrophotometric method (52.5?±?1.0 – 102?±?2.0?µg?L^?1) at 95% confidence level (t-test).     

A Resin‐Linker‐Vector Approach to Radiopharmaceuticals Containing 18F: Application in the Synthesis of O‐(2‐[18F]‐Fluoroethyl)‐L‐tyrosine

A Resin‐linker‐vector (RLV) strategy is described for the radiosynthesis of tracer molecules containing the radionuclide ¹⁸F, which releases the labelled vector into solution upon nucleophilic substitution of a polystyrene‐bound arylsulfonate linker with [¹⁸F]‐fluoride ion. Three model linker‐vector molecules 7 a – c containing different alkyl spacer groups were assembled in solution from (4‐chlorosulfonylphenyl)alkanoate esters, exploiting a lipase‐catalysed chemoselective carboxylic ester hydrolysis in the presence of the sulfonate ester as a key step. The linker‐vector systems were attached to aminomethyl polystyrene resin through amide bond formation to give RLVs 8 a – c with acetate, butyrate and hexanoate spacers, which were characterised by using magic‐angle spinning (MAS) NMR spectroscopy. On fluoridolysis, the RLVs 8 a , b containing the longer spacers were shown to be more effective in the release of the fluorinated model vector (4‐fluorobutyl)phenylcarbamic acid tert‐butyl ester ( 9 ) in NMR kinetic studies and gave superior radiochemical yields (RCY≈60 %) of the ¹⁸F‐labelled vector. The approach was applied to the synthesis of the radiopharmaceutical O‐(2‐[¹⁸F]‐fluoroethyl)‐L ‐tyrosine ([¹⁸F]‐FET), delivering protected [¹⁸F]‐FET in >90 % RCY. Acid deprotection gave [¹⁸F]‐FET in an overall RCY of 41 % from the RLV.     

Effect of post-synthetic processing conditions on structural variations and applications of bacterial cellulose

Physicochemical properties of materials can be amended by altering their physical structure through different processing conditions. The present study was conducted to investigate the post-synthesis structural variations and physico-mechanical properties of bacterial cellulose (BC) sheets prepared using different drying methods. Wet BC sheets of the same origin were freeze dried (BC-FD), dried at room temperature (25 °C) (BC-DRT), and dried at elevated temperature (50 °C) (BC-DHT). FE-SEM micrographs revealed that BC-DRT and BC-DHT had a more tightly packed and compact structure than the loosely held fibrils of BC-FD. XRD analysis revealed the relative crystallinity of the BC sample to be 64.60, 59.16, and 47.20 % for BC-DHT, BC-DRT and BC-FD, respectively. The water holding capacity (WHC) of the BC-FD was higher than that of the other two samples. Four consecutive drying and rewetting cycles demonstrated that the WHC of all samples decreased with each cycle. The WHC of BC-DRT and BC-DHT was reduced to almost 0 after the first drying cycle, but the BC-FD samples were able to regain some of their WHC. The tensile strength and elongation modulus were in the order of BC-DHT > BC-DRT > BC-FD. Overall, the results of this study revealed that the post-synthetic processing conditions had a strong effect on the structure and physico-mechanical properties of BC.