A Novel Cyclic Dinuclear Gold(I) Complex Induces Anticancer Activity via Oxidative Stress-Mediated Intrinsic Apoptotic Pathway in MDA-MB-231 Cancer Cells

A new dinuclear cyclic gold(I) complex [Au2(DCyPA)2](PF6)2, 1 based on bis[2-(dicyclohexylphosphano)ethyl]amine (DCyPA) has been synthesized and characterized by elemental analysis, IR and NMR spectroscopies, and X-ray crystallography. In the dinuclear...

Validated stability indicating RP-HPLC method for the determination of dolutegravir and rilpivirine in bulk and pharmaceutical dosage forms

For simultaneous analysis of Dolutegravir and Rilpivirine utilizing RP-HPLC, an accurate, rapid, economical, quick and reliable assay technique was developed and tested. Successful chromatographic detachment using acetonitrile and 0.1 percent tri ethyl amine in the water of pH-2.5 adjusted with 0.1% orthophosphoric acid in 40:60 v/v as a movable phase with a flow of 1 ml/min and UV observation at 230 nm. Chromatography at ambient temperature was performed isocratically, and the run time was 10 min. By injecting the norm six times, device suitability parameters were studied and the findings were far below the acceptance criteria. The linearity analysis was performed at levels ranging from 10% to 150% and the R2 value was found to be 0.999. Precision has been found to be 0.8 for repeatability and 1.2 for intermediate precision. Assay of the commercialized formulation was performed by using the above method, and we get 100.01 percent was present. For routine analysis in drug testing, this chromatographic approach can be effectively implemented. By using the above technique, an assay of the marketed formulation was performed and found to be within the limit. Degradation studies were carried out on Dolutegravir and Rilpivirine, with a purity threshold greater than purity angle in all conditions and within the acceptable range. The above-mentioned technique was validated according to ICH guidelines.

Synthesis of fused dihydrobenzo [4,5]imidazo[1,2-a]pyrmido[5,4-e]pyrmidin-3(4H)-amine derivatives

Some of fused dihydrobenzo [4,5]imidazo [1,2-a] pyrmido [5,4-e] pyrmidin-3(4H)-amine derivatives were synthesized, theses derivatives derived from 4-amino-2-(4-chloro or bromophenyl) -1,2-dihydropyrimido[1,2-a] benzimidazole-3-carbonitrile (4,5), which prepared by reaction 1H-benzimidazol-2-amine (1) and p-chlorobenzaldehyde or p-bromobenzaldehyde (2) and malononitrile (3). These derivatives prepared by reaction compound (4,5) with with triethylorthoformate in presence acetic anhydride to give the products (6,7), then the products was reacted with aliphatic amines (hydrazine, methyl amine, ethyl amine, propyl amine and isobutyl amine) to give pyrmidin rings (8-17) respectively. All these derivatives characterization by FT-IR , HNMR spectra and physical properties.

Determination of residual solvents in paclitaxel by headspace gas chromatography

Background A simple and sensitive gas chromatographic method was developed and validated for the simultaneous determination of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine in Paclitaxel. A chromatographic separation was done on DB-624 column, 30 m length × 0.53 mm ID, and film thickness 3 μm, using a flame ionization detector (FID) with gradient column oven temperature program. The injection was carried out in split mode, with a split ratio of 5:1. A mixture of N-methyl-2-pyrrolidinone (contains 1% piperazine) and water in the ratio of 80:20 (v/v) was selected as a diluent to obtain good sensitivity along with the recovery. Results The developed gas chromatographic method offers symmetric peak shape, good resolution of more than 2.0 between the solvent peaks, and the relative standard deviation for replicate injections of all the solvents were found to be not more than 15.0% with reasonable retention time for all the solvents. The limit of detection for methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 304.69 ppm, 497.98 ppm, 498.99 ppm, 504.49 ppm, 61.81 ppm, 30.07 ppm, 505 ppm, 73.05 ppm, and 2.09 ppm, respectively. Limit of quantitation of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 89.62 ppm, 146.47 ppm, 146.76 ppm, 148.38 ppm, 18.18 ppm, 8.84 ppm, 148.53 ppm, 21.49 ppm, and 0.62 ppm, respectively. Precision was found to be satisfactory. Linear in the range of LOQ to 150% level for all the solvents, and accuracy along with robustness, is performed, and acceptable results were obtained. Conclusion The proposed method was demonstrated to be simple, sensitive, specific, linear, precise, accurate, and robust, hence can be used to determine the residual organic solvents in Paclitaxel drug substance and drug product.

Synthesis, Characterization and Antimicrobial Activity Studies of Chlorocobaloximes with Neutral Bases Containing Amine Functionality

The inorganic cobaloximes of type [Co(Cl)(dmgH)2B]; where dmgH = dimethyl glyoxime and B = neutral bases: glycine, ethyl amine, 2-aminopyridine, 4-aminopyridine, 2,6-diaminopyridine, aniline and 1-napthylamine have been synthesized. The synthesized cobaloximes were characterized by IR, UV-visible, 1H NMR and 13C NMR spectroscopic techniques. The cobaloxime complexes were screened for their antibacterial activity against methicillin resistant Staphylococcus aureus (MRSA) and Acinetobacter baumannii by the zone of inhibition test, biofilm eradication on biomaterial using catheter and modified Congo red agar method. It has been found that the cobaloxime complexes exhibit inhibition against both gram positive and gram negative bacteria and the cobaloximes showed better inhibition towards Gram-negative bacteria compared to Gram-positive bacteria.

Optimization of signal amplification by reversible exchange for polarization of tridentate chelating bis[(2-pyridyl)alkyl]amine

SABRE was successfully applied on bis[(2-pyridyl)alkyl]amine derivatives and it showed the highest amplification on bis[(2-pyridyl)ethyl]amine. DFT studies with AIM analysis reveal the mechanism of hyperpolarization transfer via SABRE.