Immobilization of Urease on (HEMA/IA) Hydrogel Prepared by Gamma Radiation

In the present study, the copolymeric hydrogels based on 2-hydroxyethyl methacrylate (HEMA) and itaconic acid (IA) were synthesized by gamma radiation induced radical polymerization, in order to examine the potential use of these hydrogels in immobilization of Citrullus vulgaris urease. Gelation and Swelling properties of PHEMA and copolymeric P (HEMA/IA) hydrogels with different IA contents (96.5/3.5, 94.4/5.6 and 92.5/7.5 mol) were studied in a wide pH range. Initial studies of so-prepared hydrogels show interesting pH sensitivity in swelling and immobilization. C. vulgaris urease was immobilized on HEMA/IA (92.5/7.5) at 6 kGy with 41.3% retention of activity. The properties of free and immobilized urease were compared. Immobilized urease maintained a higher relative activity than free urease at both lower and higher pH levels, indicating that the immobilized urease was less sensitive to pH changes than the free urease. The K_m value of the immobilized urease was approximately 2 times higher than that of the free urease. Temperature stability was improved for immobilized enzyme. The free form exhibited a loss about 80% of activity upon incubation for 15 min at 80°C. The influence of various heavy metal ions at the concentration of l mM was improved after enzyme immobilization. The immobilization of C. vulgaris urease on HEMA/IA (92.5/7.5) at 6 kGy showed a residual activity of 47 % after 4 reuses.     

Novel Synthesis of Some Phthalazinone Derivatives

Dimethyl homophthalate condensed with isatin to give the unexpected five membered lactone 3 rather than the half ester 1 and the δ‐lactone 2 . Treatment of compound 3 with excess hydrazine hydrate afforded phthalazinone carbohydrazide 4 which represents a novel method for the synthesis of phthalazinone derivatives. The carbohydrazide 4 upon treatment with carbon disulphide afforded 1,3,4‐oxadiazole derivative 5 , which reacted with ethylchloroacetate to give the S‐alkylated product 6 . The structure of compound 3 compared with 2 was discussed using hyperchem professional (7) AM₁ calculations, X‐ray single crystal structure and complete spectral data.     

Spectrofluorimetric Determination of Oxamniquine in Dosage Forms and Spiked Human Plasma through Derivatization with 1-dimethylaminonaphthalene-5-sulphonyl chloride

A sensitive, simple and selective spectrofluorimetric method was developed for the determination of oxamniquine (OXM) in pharmaceutical formulations and biological fluids. The method is based on the reaction between the drug and 1-dimethylaminonaphthalene-5-sulphonyl chloride (dansyl chloride) in presence of 0.5 M sodium carbonate (pH 10) to yield a highly fluorescent derivative that is measured at 445 nm after excitation at 335 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence concentration plot was rectilinear over the range of 0.02–0.2 μg ml⁻¹ with a lower detection limit (LOD) of 0.007 μg ml⁻¹ and limit of quantitation (LOQ) of 0.02 μg ml⁻¹. The proposed method was successfully applied to the analysis of commercial capsules. The results obtained were in good agreement with those obtained using the official spectrophotometric method. Furthermore, the method was applied for the determination of oxamniquine in spiked human plasma, the mean % recovery (n = 4) is 97.77 ± 1.19. A proposal of the reaction pathway was presented.     

Thermolysis of symmetrical dithiobiurea and thioureidoethylthiourea derivatives

Microwave and thermal heterocyclization of N,N′‐disubstituted hydrazinecarbothioamide 1a,b and substituted thioureidoethylthioureas 2a–c as well as 1‐phenyl‐3[2‐(3‐phenylthio‐ureido)phenyl]thiourea 6 are reported. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:535–541, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10188     

Designing of Zn (II)-based novel coordination polymer (CP): Synthesis,characterization, and heavy metal removal from water

A new coordination polymer, Zn-(OC-AMAM-CO) CP, has been synthesized from Zn (II) as ionic node and 2,2′-((1,2-phenylenebis [azanediyl])bis (carbonyl))dibenzoic acid, (OC-AMAM-CO), as a new linker, where (OC-AMAM-CO) has been synthesized as an amide product through condensation reaction of phthalic acid and o-phenylenediamine. The amide product (OC-AMAM-CO) and Zn-(OC-AMAM-CO) CP were characterized via FTIR and PXRD analyses, and Zn-(OC-AMAM-CO) CP was further characterized via SEM/EDX and XPS analyses. Moreover, DFT study was performed to shed light on the both structures of (OC-AMAM-CO) and Zn-(OC-AMAM-CO). PXRD analysis revealed the successful syntheses of the new linker (OC-AMAM-CO) and Zn-(OC-AMAM-CO) CP where the new CP is crystalline. DFT study revealed that the 3D topological structure assembled through coordination, π–π stacking, and hydrogen bonding. Zn-(OC-AMAM-CO) CP was applied as an adsorbent for the removal of Cu (II) from water as it has abundant chelating groups that serve as adsorptive coordinating sites. Isotherm study revealed the obedience of Cu (II)/Zn-(OC-AMAM-CO) CP adsorption system to Langmuir modeling with adsorption capacity of about 55 mg/g. A kinetic study showed that the rate of adsorption was a pseudo-first-order type. Further, adsorption process was found to be strongly diffusion dependent.     

Activated nitriles in heterocyclic synthesis: Novel syntheses of 3H-1,2,4-triazolo-[1,5-a]pyridine derivatives

A new route for the synthesis of 3H-1,2,4-triazolo[1,5-a]pyridines 7a–j , 12a , b , and 17a , b utilizing the reaction of the hydrazones of cyanoethanoic acid hydrazide 3a , b with ylidene malononitriles 2a–e , malononitrile, and 3-aminocrotononitrile is described.