Pure Powder Form Research Articles

Eco-friendly electrochemical assay of oxytetracycline and flunixin in their veterinary injections and spiked milk samples

Two solid-contact electrochemical sensors were developed for detection of each of oxytetracycline HCl (OXY), and the co-formulated non-steroidal anti-inflammatory drug flunixin meglumine (FLU) in veterinary formulations and animal-derived food products. The designed sensors were based on a glassy carbon electrode as the substrate material and high molecular weight polyvinyl chloride (PVC) polymeric ion-sensing membranes doped with multiwalled carbon nanotubes (MWCNTs) to improve the potential stability and minimize signal drift. For determination of OXY, the sensing membrane was modified with potassium tetrakis (4-chlorophenyl) borate (K-TCPB), which was employed as a cation exchanger, and 2-hydroxypropyl-β-cyclodextrin (HP-ßCD), which was used as an ionophore. A linear response within a concentration range of 1 × 10− 6-1 × 10− 2 M with a slope of 59.47 mV/decade over a pH range of 1–5 was recorded. For the first time, two potentiometric electrodes were developed for determination of FLU, where the sensing membrane was modified with tetra dodecyl ammonium chloride (TDDAC) as an anion exchanger. A linear response within a concentration range of 1 × 10− 5-1 × 10− 2 M and a slope of -58.21 mV/decade over a pH range of 6–11 was observed. The suggested sensors were utilized for the selective determination of each drug in pure powder form, in veterinary formulations, and in spiked milk samples, with mean recoveries ranging from 98.50 to 102.10, and without any observed interference. The results acquired by the proposed sensors were statistically analyzed and compared with those acquired by the official methods, and the results showed no significant difference.Graphical

High Performance Thin Layer Chromatography (HPTLC) Analysis of Anti-Asthmatic Combination Therapy in Pharmaceutical Formulation: Assessment of the Method's Greenness and Blueness.

A cost-effective, selective, sensitive, and operational TLC-densitometric approach has been adapted for the concurrent assay of Hydroxyzine Hydrochloride (HYX), Ephedrine Hydrochloride (EPH), and Theophylline (THP) in their pure powder and pharmaceutical forms. In the innovative TLC-densitometric approach, HYX, EPH, and THP were efficaciously separated and quantified on a 60F254 silica gel stationary phase with chloroform-ammonium acetate buffer (9.5:0.5, v/v) adjusted to pH 6.5 using ammonia solution as a mobile liquid system and UV detection at 220 nm. The novel TLC method validation has been performed in line with the international conference for harmonization (ICH) standards and has been effectively used for the estimation of the researched medicines in their pharmaceutical formulations without intervention from excipients. Additionally, parameters affecting the chromatographic analysis have been investigated. The new TLC approach's functionality and greenness were appraised using three modern and automated tools, namely the Blue Applicability Grade Index (BAGI), the Analytical Greenness metric (AGREE), and the Green Analytical Procedure Index (GAPI) tools. In short, the greenness characteristics were not achieved as a result of using mandatory, non-ecofriendly solvents such as ammonia and chloroform. On the contrary, the applicability and usefulness of the novel TLC approach were attained via concurrent estimation for the three drugs using simple and straightforward procedures. Moreover, the novel TLC method outperforms previously published HPLC ones in terms of the short run time per sample and moderate pH value for the liquid system. According to the conclusions of comparisons with previously recorded TLC methods, our novel HPTLC method has the highest AGREE score, so it is the greenest HPTLC strategy. Moreover, its functionality and applicability are very appropriate because of the simultaneous assessment of three drugs in one TLC run. Furthermore, no tedious and complicated extraction and evaporation processes are prerequisites.

The Application of Cathodoluminescence (CL) for the Characterization of Blue Pigments

The combined application of Cathodoluminescence (CL) with Scanning Electron Microscopy (SEM) on paintings and painted surfaces has the potential to identify both organic and inorganic pigments on a micrometre or even nanometre scale. Additionally, the combination with Energy-Dispersive Spectrometry (EDS) allows for a more holistic, elemental, and mineralogical characterization of pigments. In addressing the need for the creation of a robust, open access database of characteristic CL spectra of pigments, a large project has been undertaken, focusing primarily on common organic and inorganic pigments. The present paper focuses on the CL characterization of 10 significant blue pigments in pure powder form: cerulean blue, Egyptian blue, Han blue, indigo, lapis lazuli, Maya blue, phthalo blue, vivianite, ultramarine blue, and zirconium blue. The CL spectra present characteristic bands for most of the pigments, allowing their secure identification, especially when combining the results with the EDS analyses. The effect of binding media and of the mixture of different pigments was also studied, via the analysis of mixtures of pigments with oil painted over canvas. Overall, both the binding medium and the mixture of pigments do not appear to create significant differences in the occurring spectra, thus allowing the identification of individual pigments. EDS and RAMAN spectra are included in order to facilitate comparison with other databases.

Development and Validation of Chromatographic Methods for Simultaneous Estimation of Aspirin and Pantoprazole Sodium in Pure and Mixture Form.

This technique is employed for the simultaneous quantification of aspirin (ASP) and pantoprazole sodium in both pure powder form and formulations. The high performance liquid chromatography (HPLC) method uses a C-18 column (250mm × 4.6mm, 5μm) with a mobile phase consisting of 0.05M disodium hydrogen phosphate and methanol in a 40:60% v/v ratio. The flow rate is maintained at 1.0mL/min. On a layer of silica gel 60F254 with an aluminum backing, the high performance thin layer chromatography (HPTLC) separation was carried out with ethyl acetate and methanol (8: 1.5v/v) as the mobile phase. With a mean recovery of 100.54% and 99.55% for ASP and PNT, respectively, quantification was accomplished using the HPLC method with UV detection at 286nm over the concentration range of 0.1-0.6g/mL for PNT and 0.4-2.4g/mL for ASP. With a mean recovery of 99.44% and 99.01% for ASP and PNT, respectively, quantification was achieved using the HPTLC method with UV detection at 298nm over the concentration range of 400-2400ng/spot for ASP and 100-600ng/spot for PNT, respectively. The methods can be used for the simultaneous determination of ASP and PNT in pure powder form and formulations as they are simple, accurate and sensitive.

Development of Novel Microwell-Based Spectrofluorimetry and High-Performance Liquid Chromatography with Fluorescence Detection Methods and High Throughput for Quantitation of Alectinib in Bulk Powder and Urine Samples

Background and Objectives: This study presents the development and validation of the 96-microwell-based spectrofluorimetric (MW-SFL) and high performance liquid chromatography (HPLC) with fluorescence detection (HPLC-FD) methods for the quantitation of alectinib (ALC) in its bulk powder form and in urine samples. Materials and Methods: The MW-SFL was based on the enhancement of the native fluorescence of ALC by the formation of micelles with the surfactant cremophor RH 40 (Cr RH 40) in aqueous media. The MW-SFL was executed in a 96-microwell plate and the relative fluorescence intensity (RFI) was recorded by utilizing a fluorescence plate reader at 450 nm after excitation at 280 nm. The HPLC-FD involved the chromatographic separation of ALC and ponatinib (PTB), as an internal standard (IS), on a C18 column and a mobile phase composed of methanol:potassium dihydrogen phosphate pH 7 (80:20, v/v) at a flow rate of 2 mL min-1. The eluted ALC and PTB were detected by utilizing a fluorescence detector set at 365 nm for excitation and 450 nm for emission. Results: Validation of the MW-SFL and HPLC-FD analytical methods was carried out in accordance with the recommendations issued by the International Council for Harmonization (ICH) for the process of validating analytical procedures. Both methods were efficaciously applied for ALC quantitation in its bulk form as well as in spiked urine; the mean recovery values were ≥86.90 and 95.45% for the MW-SFL and HPLC-FD methods, respectively. Conclusions: Both methodologies are valuable for routine use in quality control (QC) laboratories for determination of ALC in pure powder form and in human urine samples.

Is mushroom polysaccharide extract a better fat replacer than dried mushroom powder for food applications?

β-glucans found in the cell walls of mushrooms can be a beneficial food additive in replacing fat in commercial food products. Four commonly consumed mushroom species in Singapore, i.e., Pleurotus ostreatus spp., Lentinus edodes, Agaricus bisporus, and Flammulina velutipes were profiled for the β-glucan content in the lyophilized form and ultrasonicated assisted extracted form. Both forms were added into chicken patties, which were characterized for the moisture, cooking loss, texture, color, and chemically analyzed for the protein, crude fat, and fatty acid profiles with gas chromatography mass spectrometry (GC-MS). Pleurotus Ostreatus spp. had the highest β-glucan of 29.8 ± 0.7 g/100 g in the pure powder form and 15.9 ± 0.3 g/100 g from the extract. Crude fat in 100% fat substituted patties was lowest in Flammulina velutipes extract enriched patties and least in A. bisporus pure powder patties. Additionally, fat replacement with A. bisporus extract and powder forms resulted in the highest polyunsaturated fatty acid profile of 49.6 ± 1.9 mg/100 g patty and 79.9 ± 4.5 mg/100 g patty, respectively. Chicken patties with added mushroom extract were notable in retaining moisture, cooking yield and its structure. Fat substitution with mushroom powder was also conducted, satisfactory results indicated a possibility as a better fat replacer that is easily processed and an efficient alternative to β-glucan extract. With increasing demand for low fat foods with acceptable organoleptic properties, our study demonstrates that the inclusion of dry mushroom powder has the ability to mimic the "fattiness" of chicken patties.

Developing Metal Complexes for Captopril Quantification in Tablets Using Potentiometric and Conductometric Methods.

Potentiometric and conductometric methods were successfully applied to elucidate the interaction of 10 ions, viz., Cr3+, Fe3+, La2+, Th4+, Co2+, Mn2+, Pd2+, Sr2+, Ti2+, and Zr2+, with the antihypertensive drug captopril (CAP) and its role to determine CAP in pure powder and tablet forms. The ionization constant of CAP and the generated complexes' stability constants (log K) were evaluated using potentiometric and conductometric methods at 25 ± 0.1 °C and 0.05 M ionic strength (I) of NaNO3 aqueous solution, and CAP was then determined in pure powder and tablet forms. Complexes having metal:ligand ratios of 1:1, 1:2, and/or 1:3 were produced, regardless of the type of the ligand or metal ions. Both the suggested potentiometric and conductometric procedures were utilized to confirm the stoichiometry of the M-CAP binary complexes formed. These two different techniques were utilized successfully to determine CAP in pure powder and tablet forms. Using the standard addition method (SAM) based on the Gran plot, CAP was satisfactorily determined throughout the concentration range of 0.83-13.04 mg/mL (SD = 0.20, R = 0.9986 (n = 5)), with a detection limit of 0.64 mg/mL (SD = 0.20, R = 0.9986 (n = 5)). In the presence of common tablet excipients, no interferences were observed. The percentage of CAP recovered from various dosage formulations (tablets) varied from 95.88 to 99.92%.

Best Conditions for Extraction and Stripping of Iron from Chloridic Aqueous Medium

Pure iron is used as an additive for food and drugs to provide the human body with an important element which is iron. For this purpose, iron should be pure and in powder form, the extraction process can supply this type of iron. In this study, extraction of iron from an aqueous solution was done by cyclohexanone as an extractant. The parameters of extraction and stripping processes were studied and assessed the best values which give a high yield of separated iron from ore or any source of iron. For the preliminary study, three general parameters were studied and the best values are agitation time (10 min.), agitation speed (400 rpm), and temperature (30C). In the main study for the extraction process, there are four parameters were investigated and the optimum values are phase ratio (O/A) (1/1), iron concentration (conversely relationship), extractant concentration (proportional relationship), and normality (5 N). The best values for stripping process parameters are phase ratio(A/O) (1/2 – 1/1) and normality of strip solution (0.1 N). The extraction technique is very important in Pharmaceutical industries to produce different suitable metals associated with food and drugs. The extraction technique was detected as an appropriate method to separate iron and introduce it in pure powder form.

Spectrophotometric methods for determination of glimepiride and pioglitazone hydrochloride mixture and application in their pharmaceutical formulation

Simple, accurate, and precise four spectrophotometric methods were developed and validated for simultaneous determination of glimepiride and pioglitazone hydrochloride in their pharmaceutical formulation. The first spectrophotometric method was the dual-wavelength which determined glimepiride at 219.0 and 228.0 nm and pioglitazone hydrochloride at 268.0 nm. The second one is the first derivative of ratio spectra (DD1) spectrophotometry in which the peak amplitudes were used at 238.0 nm and 268.0 nm for glimepiride and pioglitazone hydrochloride, respectively. The third method is ratio subtraction in which glimepiride was determined at 228.0 nm in the presence of pioglitazone hydrochloride which was determined by extended ratio subtraction at 268.0 nm. The fourth method was the ratio difference to determine glimepiride and pioglitazone hydrochloride. Beer’s law was confirmed in the concentration range 2.50–15.00 µg mL-1, and 10.00–50.00 µg mL-1 for glimepiride and pioglitazone respectively for the four methods. The proposed methods were used to determine both drugs in their pure powdered form with mean percentage recoveries of 99.91 ± 1.117% for glimepiride and 99.76 ± 0.911% for pioglitazone hydrochloride in method (A). In method (B), the mean percentage recoveries were 100.12 ± 0.89% for glimepiride and 100.02 ± 1.06% for pioglitazone hydrochloride. In method (C) glimepiride was 100.01 ± 0.592% and 99.85 ± 0.845% for pioglitazone hydrochloride by extended ratio subtraction. And finally, in method (D) the mean percentage recoveries were 100.66 ± 0.670% for glimepiride and 99.92 ± 0.988% for pioglitazone hydrochloride. The developed methods were successfully applied for the determination of glimepiride and pioglitazone hydrochloride in pure powder and dosage form. The suggested methods were also used to determine both compounds in laboratory-prepared mixtures. The accuracy, precision, and linearity ranges of the developed methods were determined. The results obtained were compared statistically with the official method, and there was no significant difference between the proposed methods and the official method for accuracy and precision.

Evaluation of in silico and in lab sample enrichment techniques for the assessment of challengeable quaternary combination in critical ratio

A comparative study of successive spectrophotometric resolution technique for the simultaneous determination of a challengeable quaternary mixture of Chlorpheniramine maleate (CPM), Pseudoephedrine hydrochloride (PSE), Ibuprofen (IBU) and Caffeine (CAF) is presented, without preliminary physical separation steps. Several successive steps were applied on built-in spectrophotometer software utilizing zero and/or derivative and/or ratio spectra of the studied components. These methods, namely, Dual amplitude difference (DAD) as a novel method, Constant multiplication coupled with spectrum subtraction method (CM-SS), Factorized first derivative coupled with derivative transformation method (FD1 -DT) and Derivative ratio method (DD1). The calibration graphs are linear over the concentration range of 10.0–80.0 μg/mL,150.0–900.0 μg/mL, 200.0–1400.0 μg/mL and 3.0–30.0 μg/mL for CPM, PSE, IBU and CAF, respectively. The specificity of suggested methods was studied via laboratory prepared (diverse ratios) mixtures and were successfully applied for Antiflu® capsules' analysis. Moreover, sample enrichment via In Silico (via software of spectrophotometer) and In Lab (via spiking with pure sample) techniques was elected for a pharmaceutical dosage form analysis comprising CPM and PSE as minor components. Accuracy, precision and specificity were between the valid limits. Validation steps were done in accordance with the ICH guidelines. Moreover, statistical comparison was carried out between the obtained and reported results for pure powder form and no significant difference appeared.

Application of extracted β-glucan from oat for β-carotene encapsulation.

The cell walls of cereals are rich sources of polysaccharide β-glucan. In this study, the β-glucan was extracted from oat bran using the hot-water extraction method and dried in a pure powder form. The concentration of the β-glucan in the extract was determined using the l-cysteine sulfuric acid method. The results showed that the yield of β-glucan using the hot-water extraction method is the highest compared to its yield achieved by enzymatic, acid, and alkaline methods. In this paper, the usage of the β-glucan as a coating material for a water-insoluble carotenoid is considered. This study demonstrates for the first time the encapsulation of β-carotene with modified octanoic acid β-glucan. It implements to obtain a stable encapsulated polysaccharide-carotenoid system, which has been studied by a set of physicochemical methods and a cytotoxic analysis was performed on the HCT-116 cell line. The SEM image of the resulting encapsulated system is perfectly correlated with the DLS data, which has determined the size of MG capsules at 200nm. The cytotoxic analysis demonstrates that the cell viability was more than 70%, which indicates its potential using in the food industry.

In vitro assessment of cytotoxicity and anti-inflammatory properties of shilajit nutraceutical: A preliminary study

Background: Shilajit is a nutraceutical exudate found mainly in the Indian Himalayas, which is formed for centuries by the gradual decomposition of certain plants due to microbial action. It has been effectively used as a potent and safe dietary supplement, restoring the energetic balance and potentially able to prevent several diseases. Hence, the aim of the present preliminary in vitro study is to assess the cytotoxicity of shilajit extract and to comparatively evaluate the anti-inflammatory effect of shilajit and diclofenac sodium, a commonly used drug. Materials and Methodology: Shilajit was commercially procured in pure powder form which was dissolved in 10 ml of methanol and boiled for 80 min, followed by centrifugation (2500 rpm) for 10 min. The supernatant fluid thus obtained was used as an experimental solution. 25-mg diclofenac sodium was used as a control drug. The cytotoxicity of shilajit extract was assessed using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay, whereas the anti-inflammatory property of the test groups was comparatively evaluated using protein denaturation assay. Results: As the dilution of the extracts increased, the amount of cell viability was also increased, thereby showing that the diluted shilajit extract concentrations proved to be least cytotoxic. Different percentages of shilajit exhibited concentration-dependent inhibition of protein denaturation. Although shilajit extract exerted marginally better anti-inflammatory effect than diclofenac sodium, the effect being dose dependent; the protein inhibition values were not statistically significant (P > 0.05). Conclusion: Within the limitations of this in vitro preliminary study, it can be concluded that: (i) shilajit extract was found to be nontoxic when tested on L929 mouse fibroblast cell lines and (ii) the anti-inflammatory effect of shilajit was comparable to that of diclofenac sodium. Hence, this nutraceutical can be a viable alternative to conventional anti-inflammatory drugs in the field of medicine and dentistry.

Portable solid-state sensor for therapeutic monitoring of an antineoplastic drug; vinblastine in human plasma.

During cancer treatment, doses must be carefully administered and monitored to guarantee efficacy and minimize side-effects. A potentiometric sensor was developed for the direct real-time assay of a widely used antineoplastic drug (vinblastine (VB)) in plasma samples. Membrane cocktails were drop-casted over a glassy-carbon electrode coated with a lipophilic conducting polymer (polyaniline). The study investigated five cation exchangers, five plasticizers (of different polarities and dielectric constants), and four ionophores with different physicochemical characters on the sensor performance. The study substantiates a data-driven selection of the optimum membrane recipe. The latter included sodium tetraphenylborate as an ion exchanger, dioctylphthalate as a plasticizer, and hydroxypropyl-β-cyclodextrin as ionophore. The membrane proved a near-Nernstian slope of 37.5 mV per decade, a LOQ of 2.99 × 10−6 M, and a stable fast response. The selectivity study proved poor responses to common physiological ions. The developed sensor was used for the determination of VB in its pure powder form, marketed formulation, and plasma samples. The fast and direct sensor response enables a wide range of applications in quality control laboratories and clinical studies.

New spectral resolution techniques for resolving and determining the components in binary fixed-dose combinations

Four spectrophotometric approaches were performed to determine a binary combination of Phenazone and Benzocaine in pure powder form and in pharmaceutical formations. This investigation submits the application of four techniques contingent on the presence of the extended area of the spectra of one compound in the binary mixture, these methods include Absorptivity Centering (a-centering), Absorbance Subtraction (AS), Amplitude Modulation (AM) and Concentration Value (CV). The linearity range for the above-mentioned approaches was found to be 3.0–15.0 μg/mL for Benzocaine in a-centering method and 3.0–30.0 μg/mL for Benzocaine and Phenazone in other advanced methods. The four techniques were evaluated as per ICH criteria and were successfully utilized for the determination of Phenazone and Benzocaine existing in pharmaceutical formulations. All results gained by the submitted approaches were statistically compared with a previously published method, and no important differences were detected.

Study of efficiency and spectral resolution for mathematical filtration technique using novel unlimited derivative ratio and classical univariate spectrophotometric methods for the multicomponent determination-stability analysis

Six simple, sensitive and selective spectrophotometric methods based on mathematical filtration technique are presented for concurrent determination of aceclofenac (ACE) and paracetamol (PAR) in presence of their degradation products, namely; diclofenac sodium (DIC) and 4-aminophenol (4-AP), respectively without preliminary physical separation procedures. This technique consists of several consecutive steps applied on built-in spectrophotometer software utilizing zero and/or derivative and/or ratio spectra of the studied components. These methods, namely, dual wavelength (DW), induced dual wavelength (IDW), derivative subtraction (DS) coupled with constant multiplication (CM), ratio difference method (RD), constant center method (CC) and the novel introduced unlimited derivative ratio method (UDD). This novel method has a very powerful competence for the analysis of the challengeable mixtures lacking zero crossing point. The linearity, accuracy and precision ranges of these methods were determined and validated as per ICH guidelines. Moreover, the specificity was checked by analyzing synthetic mixtures of both drugs. These methods were applied for the determination of the cited drugs in pharmaceutical formulation and a statistical comparison of the obtained results was made with each other and with those of reported spectrophotometric method. The comparison of the results of pure powder form showed that there is no significant difference between the proposed methods and the reported method regarding both accuracy and precision.

Design and optimization of a luminescent Samarium complex of isoprenaline: A chemometric approach based on Factorial design and Box-Behnken response surface methodology.

A chemometrically optimized procedure has been developed for the determination of isoprenaline (ISO) in the parent substance as well as in its respective pharmaceutical preparation. It is worth mentioning that although spectroscopic determination of Isoprenaline metal complexes has been described in literature, yet, no methods for the quantification of Isoprenaline with Samarium nor any other lanthanide metal have been reported. Fractional factorial design (FFD) was implemented in the initial screening procedure of the four designated factors, namely, reaction time (RT), metal volume (MV), pH and temperature (T) followed by Response Surface Methodology (RSM) optimization tool performed by the aid of Box Behnken design (BBD).The proposed techniques are based on a multivariate approach where a complexation reaction between Isoprenaline (ISO) and Samarium III (Sm3+) metal was exploited for the first time to synthesize novel fluorescence and absorbance probes of ISO-Sm. Maximum fluorescence intensity (Y1) as well as maximum absorbance (Y2) of the produced complex were attained at λex/λem = 315/450 and λ 295 nm for spectrofluorimetric and spectrophotometric determinations, respectively, against blank solutions. Using assessment quality tools such as, Pareto charts, normal probability plots and statistical analysis of variance testing (ANOVA), significant factors were successfully indicated (p < 0.05). Furthermore, the proposed methods verified specificity and accuracy for the determination of Isoprenaline in its pure and pharmaceutical preparation using spectrofluorimetric (Technique A) and spectrophotometric (Technique B) techniques, respectively. Linearity was obtained in the range of (0.02-0.50 μg/mL) and (2-12 μg/mL) upon employing both techniques A and B, respectively. Furthermore, limit of detection (LOD) and limit of quantification (LOQ), were found to be 5.1877 ∗ 10-3 μg/mL, 0.01572 μg/mL and 0.5593 μg/mL, 1.6949 μg/mL, upon employing techniques A and B, respectively. Standard addition method was applied for both techniques. The analysis was successfully applied to the assay of pure powder and pharmaceutical dosage forms after which the corresponding mean recoveries were computed and were found to be in the range of 99.546%-100.257% (Technique A) and 99.872%-99.887% (Technique B) with RSD (<1).

Screening and optimization of samarium-assisted complexation for the determination of norfloxacin, levofloxacin and lomefloxacin in their corresponding dosage forms employing spectrofluorimetry.

Multivariate strategy was applied for setting a fluorescent technique for the determination of three fluoroquinolones: norfloxacin (NOR), levofloxacin (LEV) and lomefloxacin (LOM) in their pure powder and dosage forms. Based on their known interaction with lanthanides, and augmented fluorescence intensity obtained by antenna effect at λex/λem = 314/553, 312/553 and 310/556 for NOR, LEV and LOM, respectively, the current research was scrutinized. Four continuous factors were selected for study in the screening step by means of Plackett-Burman Design, where temperature factor was excluded for being non-significant and the other factors as volume of metal ion solution, pH and reaction time were evaluated through Central Composite Design. 3-D surfaces demonstrations and 2-D contour plots designated the factors interactions followed by optimization plots, which defined the best blend for factors conjunction. pH factor was the chief motor force affecting the response as the number of coordinated ligands formed depends on the pH, whereas 1:2 complex is the main species at higher pH values followed by the volume of metal ion solution and ended by little effect of the reaction time. Model verification was monitored, which showed the model superiority for the three fluoroquinolones, where all target points tested were in good agreement with the predicted ones. The linear range for the tested drugs were found to be 0.090-1.280 μg/mL for NOR, 0.068-1.448 μg/mL for LEV and 0.077-1.552 μg/mL in case of LOM, thus approving the suitability of this method for Quality Control testing. Furthermore, applying these conditions to test the fluoroquinolones in their pharmaceuticals was done as well as intra and inter-day effects as to confirm the validity of this technique for routine analysis. Recovery % and RSD were found to be 99.958 ± 0.797, 99.887 ± 0.935 and 100.427 ± 0.698 for NOR, LEV and LOM respectively in their pure powder. While it was calculated to be 100.200 ± 0.785, 100.530 ± 0.396 and 100.620 ± 0.896 for NOR, LEV and LOM in their corresponding dosage forms. This excellent precision and accuracy obtained in results impulse it to be one of the most appropriate methods for further analysis.

Direct Synthesis of Iron Oxide (α-Fe2O3) Nanoparticles by the Combustion Approach

A facile and rapid combustion method was developed to synthesis to produce iron oxide (α-Fe2O3) nanopowder using dissolution of iron nitrate (as the oxidant) and glycine (as fuel) as the starting materials. Generally, combustion synthesis of different oxides involves a self-sustained reaction between a metal nitrates (oxidizer) and a urea, glycine, citric acid, hydrazine (fuel). Stoichiometric amounts of iron nitrate and glycine were dissolved in deionized water and poured into a quartz container can be mixed well by magnetic stirring for 1/2 h, which makes them almost as homogeneous mixtures, which was placed in a furnace at 300 °C. Initially, the solution boils and undergoes dehydration followed by decomposition with the evolution of large amount of gases with white fumes coming out from the exhaust opening provided on the top of the furnace in 15 minutes. After the solution reaches the point of spontaneous combustion, it begins burning and releases lots of heat, vaporizes all the solution instantly and becomes a foamy white solid powder. X-ray diffraction studies confirmed that the resultant powder with well-crystalline structure of pure α-Fe2O3 are produced using a single approach while simultaneously avoiding additional calcination procedures. Morphological analysis of the spherical structure of nanoparticle was achieved by SEM analyses is in the range of 35 nm and the study of the chemical the Fe2O3 bonds created was made possible by FTIR analysis. The XRD, FTIR and Raman spectra confirmed the formation of rhombohedral structural α-Fe2O3. Overall glycine-nitrate combustion synthesis has an outstanding potential for producing pure powder form of α-Fe2O3 nano particles, which leads to use in applications require high strength crystalline material.

Chromatographic Study of Azintamide in Bulk Powder and in Pharmaceutical Formulation in the Presence of Its Degradation Form.

Two specific, sensitive, and precise stability-indicating chromatographic methods were developed, optimized, and validated for the determination of Azintamide (AZ) in the presence of its degradation product. The first method was TLC combined with the densitometric determination of the separated bands. Separation was achieved using silica gel 60 F254 TLC plates and chloroform-acetone-glacial acetic acid (7.5 + 2.1 + 0.4, v/v/v) as the developing system. Good correlations were obtained between the integrated peak area of the studied drug and its corresponding concentrations in the linearity range. The second method used HPLC with UV diode-array detection, in which the proposed method was applied for the quantitative determination of AZ in the presence of its acidic degradation product and the quantitative determination of the acid-induced degradation product of AZ (AZ Deg) using pentoxifylline as the internal standard. The proposed components were separated on a reversed-phase C18 analytical column using acetonitrile-water (50 + 50, v/v). The flow rate was maintained at 0.55 mL/min and the detection wavelength was 260 nm. Linear regressions were obtained in the range of 1-30 and 0.3-16 μg/mL for AZ and AZ Deg, respectively. Different parameters affecting the suggested methods were optimized for maximum separation of the cited components. The suggested methods were validated in compliance with the International Conference on Harmonization guidelines and successfully applied for the determination of AZ in its pure powder form and in its pharmaceutical formulation. Both methods were also statistically compared with the reported method with no significant difference in performance observed.

Enhanced spectrofluorimetric determination of the multitargeted tyrosine kinase inhibitor, crizotinib, in human plasma via micelle-mediated approach

Purpose: To quantify the multi-targeted tyrosine kinase inhibitor, crizotinib, in human plasma and bulk powder by highly sensitive micellar enhanced spectrofluorimetric procedure. Method: The developed procedure was based on measuring the fluorescence intensity of crizotinib (CRZ) in sodium dodecyl sulphate (SDS) micellar system at 404 nm after excitation at 271 nm. Validation of the developed procedure was carried out following ICH (International Council for Harmonization) guidelines. Results: Maximum fluorescence intensity (FI) was attained by addition of 0.2 mL SDS and 0.2 mL HCl (1N) to CRZ aliquots and then dilution with distilled water. There was a linear relationship between the FI of CRZ and its concentration over the range, 5 – 400 ng/mL, with limit of detection and of quantification of 1.857 and 5.628 ng/mL respectively. The developed procedure was successfully applied to assay CRZ in pure powder form and spiked human plasma with mean recovery of 100.68 ± 0.37 and 99.98 ± 0.20 %, respectively. Conclusion: The developed procedure is simple and sensitive, and can be applied to routine analysis of CRZ in pure powder form as well as in clinical laboratories for the determination of CRZ in plasma. Keywords: Crizotinib, Spectrofluorimetry, Micelle, Human plasma, Sodium dodecyl sulphate