Ternary metal complexes of guaifenesin drug: Synthesis, spectroscopic characterization and in vitro anticancer activity of the metal complexes.

The coordination behavior of a series of transition metal ions named Cr(III), Fe(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) with a mono negative tridentate guaifenesin ligand (GFS) (OOO donation sites) and 1,10-phenanthroline (Phen) is reported. The metal complexes are characterized based on elemental analyses, IR, (1)H NMR, solid reflectance, magnetic moment, molar conductance, UV-vis spectral studies, mass spectroscopy, ESR, XRD and thermal analysis (TG and DTG). The ternary metal complexes were found to have the formulae of [M(GFS)(Phen)Cl]Cl·nH2O (M=Cr(III) (n=1) and Fe(III) (n=0)), [M(GFS)(Phen)Cl]·nH2O (M=Mn(II) (n=0), Zn(II) (n=0) and Cu(II) (n=3)) and [M(GFS)(Phen)(H2O)]Cl·nH2O (M=Co(II) (n=0), Ni(II) (n=0) and Cd(II) (n=4)). All the chelates are found to have octahedral geometrical structures. The ligand and its ternary chelates are subjected to thermal analyses (TG and DTG). The GFS ligand, in comparison to its ternary metal complexes also was screened for their antibacterial activity on gram positive bacteria (Bacillus subtilis and Staphylococcus aureus), gram negative bacteria (Escherichia coli and Neisseria gonorrhoeae) and for in vitro antifungal activity against (Candida albicans). The activity data show that the metal complexes have antibacterial and antifungal activity more than the parent GFS ligand. The complexes were also screened for its in vitro anticancer activity against the Breast cell line (MFC7) and the results obtained show that they exhibit a considerable anticancer activity.

Correlation between ionic radii of metal azodye complexes and electrical conductivity.

5-(2,3-Dimethyl-1-phenylpyrazol-5-one azo)-2-thioxo-4-thiazolidinone (HL) and its metal complexes with copper(II) (1), cobalt(II) (2) and nickel(II) (3) are synthesized and characterized by physico-chemical techniques. The thermal properties of the ligand (HL) and its metal complexes (1-3) are discussed. The thermal activation energies of decomposition (Ea) of HL and its metal complexes with Cu(II), Co(II) and Ni(II) are found to be 48.76, 36.83, 30.59 and 40.45 kJ/mol, respectively. The frequency and temperature dependence of ac conductivity, dielectric constants for HL and its complexes (1-3) are investigated in the temperature range 300-356 K and frequency range 0.1-100 kHz. Both of the ac conductivity and the values of the thermal activation energy for conduction, as well as the dielectric properties of the complexes of HL are found to depend on the nature of the metallic ions. The values of the thermal activation energies of electrical conductivity decrease with increasing the value of test frequency. The small polarons tunneling (SPT) is the dominant conduction mechanism for the ligand (HL), while for complex (2) the overlapping large tunneling model (OLPT) is the dominant conduction mechanism. The correlated barrier hopping (CBH) is the dominant conduction mechanism for both of the complexes (1) and (3).

Symptoms and quadriceps fatigability after walking and cycling in chronic obstructive pulmonary disease.

Patients with chronic obstructive pulmonary disease (COPD) may stop cycling due to leg effort rather than breathlessness. However, cycling is not relevant to many patients, although walking may be more familiar. A total of 84 patients with COPD were asked to name the predominant symptom limiting incremental shuttle walking, endurance shuttle walking, incremental cycle ergometry, and endurance cycle ergometry, performed to exhaustion on four separate days. Furthermore, quadriceps fatigability was evaluated in 12 patients by measuring unpotentiated and potentiated twitch quadriceps tensions before and 30 minutes after incremental walking and cycling. Breathlessness alone was a more commonly cited limiting symptom after incremental walking compared with incremental cycling (81 vs. 34%; p < 0.001) and after endurance walking compared with endurance cycling (75 vs. 29%; p < 0.001). In addition, there was no significant change in mean pre- and postwalking twitch quadriceps tensions. However, cycling produced a significant reduction (unpotentiated 7.42 +/- 2.22 vs. 6.48 +/- 2.09 kg [p < 0.001]; potentiated 10.19 +/- 3.99 vs. 8.45 +/- 3.18 kg [p < 0.001]). Pre- to postexercise changes were significantly greater during cycling compared with walking (unpotentiated p = 0.01; potentiated p = 0.003). Leg effort is an infrequent symptom after walking in COPD, and low frequency fatigue of the quadriceps is an infrequent feature of incremental walking.

2,6-Dichloroquinone chlorimide and 7,7,8,8-tetracyanoquinodimethane reagents for the spectrophotometric determination of salbutamol in pure and dosage forms.

A simple, rapid and sensitive spectrophotometric method for the determination of sulbutamol in pure form and in different pharmaceutical preparations has been developed. The charge transfer (CT) reaction between salbutamol as electron donor and 2,6-dichloroquinone chlorimide (DCQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as a pi-electron acceptor have been spectrophotometrically studied. The optimum experimental conditions for these CT reactions have been studied carefully. Beer's law is obeyed over the concentration range of 1.0-30.0 microg ml(-1) and 2.0-20.0 microg ml(-1) for salbutamol using DCQ and TCNQ, respectively. For more accurate results, Ringbom optimum concentration range is calculated and found to be 10.0 to 30.0 and 8.0 to 20 microg ml(-1) for salbutamol using DCQ and TCNQ, respectively. The Sandell sensitivity is found to be 0.011 and 0.010 g cm(-2) for salbutamol using DCQ and TCNQ, respectively, which indicate the high sensitivity of the proposed methods. Relative standard deviations (R.S.D.) of 0.27 to 0.68% and 0.20 to 1.40% (n=5) were obtained for five replicates of salbutamol using DCQ and TCNQ, respectively. The results obtained by the two reagents are comparable with those obtained by British pharmacopoeia assay for the determination of salbutamol in raw materials and in pharmaceutical preparations.

Thermal and kinetic studies on solid complexes of 2-(2-benzimidazolylazo)-4-acetamidophenol with some transition metals.

The preparation and characterization of 2-(2-benzimidazolylazo)-4-acetamidophenol (BIAAP) complexes are reported. Different physico-chemical methods like IR, Magnetic, solid reflectance spectra and molar conductance, were used to investigate the structure of BIAAP complexes. In particular, the thermal decomposition of Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes of BIAAP is studied in nitrogen atmosphere. All the complexes do not contain coordinated water molecules but contain (2-4) water molecules of crystallization. The water molecules were removed in a single step. The complexes of Co(II) and Ni(II) ions exhibited a phase transition and the decomposition or combustion of BIAAP occurred in the second and subsequent steps. The final decomposition products were identified by mass spectrometry as the corresponding metal oxides or carbonate. The activation thermodynamic parameters, such as, energy of activation, enthalpy, entropy and free energy change of the complexes were evaluated and the stabilities of the thermal decomposition of the complexes are discussed. From the kinetic point of view, it is found that the thermal stability of the complexes follows the order Ni(II) > Cu(II) > Zn(II) > Fe(III) > Co(II) > Cd(II).

Metal complexes of antibiotic drugs. Studies on dicluxacillin complexes of FeII, FeIII, CoII NiII and CuII.

The synthesis and characterization of dicluxacillin (DC) complexes with di- and tri-valent metal ions are described. The nature of bonding of the chelated DC and its metal complexes structures have been elucidated on the basis of their spectroscopic (infrared, solid reflectance, magnetic spectra, mass and thermal analysis) properties. In all the complexes studied, the DC acts as a chelate monoanionic ligand with coordination involving the carboxylate O atom and the endocyclic N of the thiazole ring. The DC ligand forms mono-ligand complexes of the general formula [M(DC)(H2O)x(A)]. yH2O where DC is the uninegatively charged bidentate ligand and A = OAc in case of CuII and Cl in case of FeIII, FeII, CoII and NiII ions. IR, solid reflectance spectra and magnetic moment measurement are used to infer the structure and to illustrate the coordinating capacity of the ligand. From the thermal decomposition curves, the water molecules of crystallization are removed in a single stage while the decomposition of the ligand and coordinated water molecules occur in the second and subsequent stages. Different thermodynamic kinetic parameters namely activation energy (E*), enthalpy of activation (AH*), entropy of activation (AS*) and free energy change of activation (AG*) are calculated using Coats and Redfern equation.

Thermodynamic and multinuclear magnetic resonance study of dimethyltin (IV) complexes with some imidazoles in aqueous solutions.

The interaction between imidazole (L1), 2-isopropylimidazole (L2), 2-amino-benzimidazole (L3) and 2-(2-pyridyl)benzimidazole (L4) (L in general), and dimethyltin chloride in water have been investigated at 25 degrees C and ionic strength of 0.1 M sodium nitrate using the potentiometric technique. The results showed the formation of 1:1 and 1:2 (organotin:ligand) complexes and the corresponding stability constants were determined. The effect of the pKa values of the respective ligands on the stability constants of its complex species was elucidated. The concentration distribution of the complexes in solution was evaluated. Also, their solid complexes of the general formula in diethylether-dichloromethane, give 1:2 (organotin:Ligand) [(L)2 (CH3)2 SnCl2.zH2O][L = L1, z = 0 and L = L2, z = 1] and 1:1 [L (CH3)2 SnCl2.zH2O][L = L3, z = 0 and L = L4, z = 2]. The separated solid products were characterized by elemental analyses (C, H, N, Cl), IR, mass spectra, thermogravimetric analysis (TGA) and magnetic susceptibility. The participation of the ligand functional groups in bonding to the organotin (IV) was discussed. Conductivity and 1H-NMR spectra were used to confirm the behaviour of these complexes in solution.

Structural chemistry of some new azo complexes.

The preparation of 2-thiouracil (H2L) and its 5-(2-thiazolylazo)thiouracil (H2L') complexes with CoII, NiII, CuII, ZnII and CdII are reported. The new complexes have been characterized by elemental analyses, solid reflectance, infrared spectra and magnetic susceptibilities. These measurements suggest that, the ligand is bound to the metal ion through nitrogen and/or sulphur atom behaving as mono- or bidentate ligand. Thermal decomposition studies of these metal complexes are explained to give more information on the structure of the investigated chelates. On the basis of the v(OH) bending frequencies and the insolubility of the complexes in common organic solvents, polymeric structures have been proposed.

Spectrophotometric determination of ampicillin, dicluxacillin, flucloxacillin and amoxicillin antibiotic drugs: ion-pair formation with molybdenum and thiocyanate.

A sensitive spectrophotometric method is developed for the determination of some antibiotic drugs such as ampicillin (amp), dicluxacillin (dicl), flucloxacillin (fluc) and amoxicillin (amox). The method involves the formation of ion-pairs between these drugs under investigation and inorganic complex of Mo (V) thiocyanate followed by its extraction with methylene chloride. The optimum conditions for the ion-pairs formation are established. The method permits the determination of amp, dicl, fluc and amox over a concentration range of 1.5-77.5, 3-75, 1.5-79 and 7.5-75 microg ml(-1) respectively. The sensitivity (S) is found to be 0.017, 0.061, 0.014 and 0.073 microg cm(-2) for amp, dicl, fluc and amox, respectively. The method is simple, rapid, reproducible and accurate within +/- 1%. The method is applicable for the assay of the four drugs under investigation in different dosage forms and the results are in good agreement with those obtained by the official method.

Spectral and thermal studies of thiobarbituric acid complexes.

The complexes of 2-thiobarbituric acid with Fe(II), Fe(III), Co(II), Cu(II), Zn(II) and Cd(II) have been isolated and characterized on the basis of elemental analyses, molar conductance, magnetic moment and spectral studies. The thermal decomposition of the metal complexes was studied by TG and DTA techniques. The kinetic parameters namely, activation energy, entropy of activation and the reaction orders were estimated.