Essential (volatile) oil from leaves of Artemisia monosperma L. belonging to family Asteraceae, and aerial parts of Tamarix aphylla L. (Athel) belonging to family Tamaricaceae were collected from the desert of Ha'il region, northern region of Saudi Arabia, hydro distilled by Clevenger apparatus and analysed by means of GC-MS techniques. Antioxidant activities of essential oils of A. monosperma and T. aphylla compared with ascorbic acid and butylated hydroxytoluene (BHT) as reference antioxidant compound were determined by method of DPPH radical scavenging assay and ABTS assay. In vitro screening of potential cytotoxicity of essential oils was also evaluated against human promyelocytic leukaemia cell lines (HL60 and NB4). The GC/MS analysis of A. monosperma essential oil resulted in identification of 61 components predominated mainly by β-Pinene as principal component (29.87%) and T. aphylla resulted in identification of 37 components of essential oil predominated mainly by 6,10,14- trimethyl-2-pentadecanone (21.43%) as principal component. Antioxidant activity as 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging and 2,2 -azino-bis (3-ethylbenzothiazoline-6-sulfonic acid (ABTS) increased with increasing essential oil concentrations of A. monosperma and T. aphylla (25, 50, 75, 100 and 200 μg mL-1). The most pronounced increases detected in the high concentrations of the two essential oils. Biologically, essential oil extracts exhibited cytotoxicity effects in dose dependent manner against human promyelocytic leukaemia cell lines (HL60 and NB4). In conclusion, A. monosperma and T. aphylla essential oils could be valuable source for cytotoxic agents with high safety and selective cytotoxicity profiles.
A simple and sensitive bioanalytical high-performance liquid chromatographic method with ultraviolet detection was developed and validated for the quantification of febuxostat (FEB) in human plasma. Ketoprofen was used as an internal standard. The analytes were extracted from human plasma samples by precipitation with acetonitrile. The reconstituted samples were chromatographed on C18 Bondapack 10 µm, 250 × 4.6 mm, Waters Column (Ireland) by using a mixture of acetonitrile and 0.5% aqueous phosphoric acid (pH 3) (52 : 48, v/v) as the mobile phase. The chromatographic separation was isocratically performed at room temperature at a flow rate of 1.0 mL/min with UV detection at 315 nm. The method exhibited a linear dynamic range over 0.05-5.00 µg/mL FEB in human plasma. The lower limit of quantification was 0.05 µg/mL. The results of the intra- and interday precision and accuracy studies were within the acceptable limits. The validated method was successfully applied for the determination of FEB in human plasma samples for application in bioequivalence studies.
KEYWORDSThree different spectrophotometric methods are developed for the determination of naftidrofuryl oxalate (NAF) in pure form and its pharmaceutical preparation. The methods are based on charge transfer complexation reactions of NAF as n-electron donor with either p-chloranilic acid (PCA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) or tetracyano ethylene (TCNE) as π-receptors to give highly colored anion radicals species. The colored products were quantified spectrophotometrically at 515, 588 and 396 nm in PCA, DDQ and TCNE methods, respectively. Under the optimized experimental conditions, Beer's law is obeyed over the concentration ranges of 75.0-300.0, 25.0-150.0 and 15.0-50.0 μg/mL NAF for PCA, DDQ and TCNE methods, respectively. The proposed methods were applied successfully to the determination of NAF in pure form and its commercial tablets with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and Fratio at 95% confidence level, showing that there is no significant difference between the reference and the proposed methods with regard to accuracy and precision. Further, the validity of the proposed methods was confirmed by standard addition technique.Chloranilic acid Tetracyanoethylene Naftidrofuryl oxalate Pharmaceutical preparation Charge transfer complexation 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone
A rapid, simple, and selective method was developed for the determination of etodolac. The method depends on complexation of etodolac with copper (II) acetate and iron (III) chloride followed by extraction of complexes with dichloromethane and then measuring the extracted complexes spectrophotometrically at 684 and 385 nm in case of Cu (II) or Fe (III), respectively. Different factors affecting the reaction, such as pH, reagent concentration, and time, were studied. By use of Job's method of continuous variation, the molar ratio method, and elemental analysis, the stoichiometry of the reaction was found to be in the ratio of 1:2 and 1:3, metal:drug in the case of Cu (II) and Fe (III), respectively. The method obeys Beer's law in a concentration range of 2.00–9.00 and 0.50–2.00 mg/mL in case of Cu (II) and Fe (III), respectively. The stability of the complexes formed was also studied, and the reaction products were isolated for further investigation. The complexes have apparent molar absorptivities of about 32.14 ± 0.97 and 168.32 ± 1.12 for Cu (II) and Fe (III), respectively. The suggested procedures were successfully applied to the analysis of pure etodolac and its pharmaceutical formulations. The validity of the procedures was further ascertained by the method of standard additions, and the results were compared with other reported spectrophotometric methods and showed no significant difference in accuracy and precision.
The aim of the present study was to assess in vitro the antiradical and antioxidant activities of successive extracts and semi-purified fractions from Rumex vesicarius L. In the present work, three extracts (n-Hexane, ethyl acetate and methanol) and 22 column fractions of methanolic extract (as promising extract) were evaluated against 2,2-diphenyl- 1-picrylhydrazyl (DPPH•) and 2,2-azinobis (3-ethylbenzothiazoline- 6-sulfonic acid) (ABTS) radical scavenging methods as antiradical and antioxidant activities compared with Butylated hydroxytoluene (BHT) as synthetic standard and silver nanoparticles of methanolic extract (Ag-NPs-Me), in addition to analysis of chemical constituents of extract and fraction using Gas chromatography–mass spectrometry (GC-MS). The obtained results revealed that, both methods go parallel showing that the concentration of extract and incubation time are dependent and proportional with phenolic compounds concentration. Absolute methanol extract recorded the highest antioxidant activity when compared with the other crude extracts with 79.3 and 78.8% against DPPH and ABTS respectively when compared with BHT as synthetic standard (89.4 and 89.9%) against DPPH and ABTS respectively. Calculation of the antiradical activity units showed the highest values of methanolic extract and its promising fraction (No. 12) after 300 seconds (5 minutes) comparing with antioxidant activity (30 min). Also, the antioxidant activity increased with synthetic Ag-NPs-Me when compared with methanolic extract by (IC50= 53.9 and 74.6 µg/ml respectively). Thus, the GC-MS analysis of successive extracts of R. vesicarius L showed a highly complex profile, containing approximately 24 different components. One pure compound was identified from fraction No. 12. The identified compound was l-(+)- ascorbic acid 2, 6-dihexadecanoate. The data also revealed presence of closely similar antioxidant activities in methanolic extract or its pure compounds with BHT when mixed at different proportions. From the obtained results it could be concluded that R. vesicarius methanolic extracts and fractions can be extensively used in the production of potential antioxidant, antiradical and AgNPs-Me for biomedical application on the consumer’s health.
Three polyvinylchloride (PVC) membrane sensors for the determination of moexipril hydrochloride were prepared and characterized. The sensors are based on the use of the ion association complexes of moexipril cation with either ammonium reineckate (sensor 1) or tetraphenyl borate (sensor 2) or phosphotungistic acid (sensor 3) counter anions as ion exchange sites in the PVC matrix. The performance characteristics of these sensors were evaluated according to IUPAC recommendations, which reveal a fast, stable and linear response for moexipril over the concentration range of 10 -6 to 10 -2 M for the three sensors with cationic slopes of 29.1, 30.1 and 30.2 mV per concentration decade for the three sensors, respectively. The direct potentiometric determination of moexipril hydrochloride using the proposed sensors gave recoveries % of 99.64 ± 0.34, 99.34 ± 0.56 and 99.68 ± 0.42 for the three sensors, respectively. The sensors were used for determination of moexipril hydrochloride in pharmaceutical formulations and in plasma. Validation of the method shows suitability of the proposed sensors for use in quality control assessment of moexipril hydrochloride. The obtained results were in a good agreement with those obtained using the reported spectrophotometric method.
Rhanterium epapposum, native to the Arabian Peninsula, is traditionally used to cure skin infections. The objective is to screen the phytochemical content and antimicrobial activity of aqueous, methanol and 80% methanol extracts of aerial parts of R. epapposum. The phytochemical screening of aqueous, methanolic, and 80% methanol extracts of R. epapposum was conducted using gas chromatographymass spectrometry. The antimicrobial activities of the extracts were assessed by well diffusion and microdilution methods. Qualitative phytochemical analysis revealed the presence of 2-methoxy-4-vinylphenol in all three extracts, whereas ethanol, 2-methoxy-, acetate; n-hexadecanoic acid; and 2,3-butanediol are present in higher amount exclusively in the methanol, 80% methanol and aqueous extracts of the aerial parts of R. epapposum, respectively. The highest antibacterial activity was shown by the aqueous extract S. aureus, P. aeruginosa, E. cloacae, and K. pneumoniae, methanolic extract against S. aureus, methicillin-resistant S. aureus, and E. coli, and 80% methanol extract against S. epidermidis, and S. paucimobilis. Interestingly, 80% methanol extracts showed the highest antifungal activity against C. albicans, C. guillermondii, C. vaginalis, C. utilis, and C. tropicalis. The aerial parts of R. epapposum showed broad-spread antimicrobial activity against bacteria and fungi. Especially, the 80% methanol extract showed potent antifungal activity against all the tested fungal strains.
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