Validated spectrofluorimetric assay of two co-administered drug mixtures containing hydroxychloroquine with either moxifloxacin or ofloxacin as a drug regimen for hospital-acquired pneumonia in patients with COVID-19.

Moxifloxacin and ofloxacin are two broad-spectrum quinolone antibiotics. They are among the most widely used antibiotics, at this time, applied to control the COVID-19 pandemic. Hydroxychloroquine is an FDA-approved drug for the treatment of COVID-19. This work describes a simple, green, selective, and sensitive spectrofluorimetric method for the assay of moxifloxacin and ofloxacin in the presence of hydroxychloroquine, two co-administered mixtures used in the treatment of hospital-acquired pneumonia in patients with COVID-19. Simultaneous assay of hydroxychloroquine and moxifloxacin was carried out in methanol using a direct spectrofluorimetric method (method I) at 375 and 550 nm, respectively, after excitation at 300 nm. The direct spectrofluorimetric assay was rectilinear over concentration ranges 50.0-400.0 and 300.0-2500.0 ng/ml for hydroxychloroquine and moxifloxacin, respectively, with limits of detection (LOD) of 6.4 and 33.64 ng/ml and limits of quantitation (LOQ) of 19.4 and 102.6 ng/ml, respectively, for the two drugs. The assay for hydroxychloroquine and ofloxacin was carried out by measuring the first derivative synchronous amplitude for hydroxychloroquine at the zero crossing point of ofloxacin and vice versa at Δλ = 140 nm (method II). Hydroxychloroquine was measured at 266 nm, while ofloxacin was measured at 340 nm over the concentration range 4-40 ng/ml for hydroxychloroquine and 200-2000 ng/ml for ofloxacin with LOD of 0.467 and 25.3 ng/ml and LOQ of 1.42 and 76.6 ng/ml, respectively, for the two drugs. The two methods were validated following International Conference on Harmonization guidelines and were applied to the analysis of the two drugs in plasma with good percentage recoveries (109.73-93.17%).

First-derivative synchronous spectrofluorimetric method for estimation of losartan potassium and atorvastatin in their pure forms and in tablets.

Losartan potassium (LOS) and atorvastatin (ATR) are used in combination for long-term treatment of stroke and for treatment of hypertension with high-level cholesterol. Both drugs were simultaneously determined and validated using a novel, easy, fast, and economical first-derivative synchronous fluorescence spectroscopic method. Methanol was used as the solvent for both drugs at a Δλ 80 nm and with a scanning rate of 600 nm/min. Peaks were determined as at 288.1 nm and 263.6 nm for LOS and ATR, respectively. The proposed method was validated according to International Conference on Harmonization guidelines and, subsequently, the developed method was applicable to the analysis of the two compounds in their different formulations without interference from each other. Amplitude-concentration plots were rectilinear over the concentration ranges 1.0-10.0 µg/ml and 0.5-5.0 µg/ml for LOS and ATR, respectively. Detection limits were found to be 0.096 µg/ml and 0.030 µg/ml and quantitation limits were 0.291 µg/ml and 0.093 µg/ml for LOS and ATR, respectively. The proposed method was successfully applied to the analysis of both compounds in synthetic mixtures and in laboratory-prepared tablets. These results were in accordance with the results acquired using the comparison method, high-performance liquid chromatography.

Two validated spectrofluorimeteric and high performance liquid chromatography (HPLC) methods with fluorescence detection for the analysis of a new anti-hepatitis C drug, daclatasvir hydrochloride, in raw material or tablet form and in biological fluids.

Two sensitive and accurate methods have been developed for the estimation of daclatasvir (DAC) in its raw material, dosage form and in biological fluids. Method I is based on the measurement of DAC native fluorescence in methanol at 385 nm after excitation at 315 nm. The relationship between fluorescence intensity and concentration was found to be rectilinear over the linearity range (3.0-30.0 ng/ml). There were good per cent recoveries both in the dosage form (99.87 ± 0.84) and in spiked human plasma (99.96 ± 1.54%). Method II utilized reversed-phase high performance liquid chromatography to estimate the antiviral agent daclatasvir hydrochloride against hepatitis C within 4.0 min on a C18 column (Eurosphere. 100-5 C18, 150 × 4.6 mm, Germany) using a mobile phase consisting of acetonitrile and 0.1 M sodium dihydrogen phosphate (30:70, v/v) at pH 3.0 and with a fluorescence detector adjusted to 315 nm and 385 nm for excitation and emission respectively. The calibration curve was linear over the range (20.0-200.0 ng/ml) with SD 1.38%, error 0.56%, recovery 99.99 ± 1.30% in tablets, recovery 100.28 ± 1.73% in spiked urine and recovery 99.63 ± 2.72% in spiked plasma.The new developed methods were successfully applied to the assay of the daclatasvir in tablet form and extended to its determination in real plasma, spiked human plasma and urine. The analytical performance of the proposed method was validated according to International Conference on Harmonization (ICH) guidelines. The proposed methods were compared with the results of a comparison method and it was found that there was no significant difference between the methods, as revealed by Student's t-test and variance ratio F-test.

Green micellar HPLC analysis of three angiotensin-converting enzyme inhibitors in their mixtures with hydrochlorothiazide and modeling of their retention behavior by fitting to Foley's model.

We present an environmentally friendly method for the analysis of three angiotensin-converting enzyme inhibitors and hydrochlorothiazide simultaneously using a green micellar eluent for the first time. The chromatographic separation of enalapril maleate, lisinopril dihydrate, benazepril hydrochloride, and hydrochlorothiazide was implemented on an octadecyl silica column with a solution containing sodium dodecyl sulfate (0.12 M), 1-propyl alcohol (10% v/v), triethylamine (0.3% v/v), and H3 PO4 (0.02 M) at pH 3.6 as the mobile phase and UV detection at 210 nm. Validity of the method was confirmed and it exhibited good linearity within the ranges of 5.0-50.0 µg/mL for hydrochlorothiazide and 10.0-60.0 µg/mL for the three angiotensin-converting enzyme inhibitors with a limit of detection of 0.39 to 1.15 µg/mL for all the studied drugs. The developed micellar high-performance liquid chromatography method enables the quantification of the targeted angiotensin-converting enzyme inhibitors in combined tablets with hydrochlorothiazide by isocratic elution. There is no need for special precautions to prevent broadening and splitting of their chromatographic peaks. The method fulfills the society rights for safe and green analytical methods. The retention behavior of the four studied drugs was fitted to Foley's model and their association equilibria to the micelles (KAM ) and to the surface-modified stationary phase (KAS ) were calculated.

Simultaneous determination of metolazone and losartan potassium in their binary mixtures using high-performance liquid chromatography with fluorimetric detection: application to combined tablets and spiked human plasma.

A new, specific and sensitive reversed-phase high-performance liquid chromatography method was developed for the simultaneous determination of metolazone (MET) and losartan potassium (LOS). Good chromatographic separation was achieved within 6.0 min on a 150 × 4.6 mm i.d., 5 µm Waters, Ireland and ProDIGY 5 ODS 3 100 A column. A mobile phase containing a mixture of methanol and 0.02 M phosphate buffer (65:35, v/v) at pH 3.0 was used. The analysis was performed at a flow rate of 1 mL/min with fluorescence detection at 410 nm after excitation at 230 nm. Aspirin (ASP) was used as an internal standard. The proposed method was rectilinear over 2.0-40.0 (MET) and 40.0-800.0 ng/mL (LOS), with limits of detection of 0.22 and 4.52 ng/mL and limits of quantification of 0.68 and 13.70 ng/mL for MET and LOS, respectively. The method was successfully applied for the simultaneous analysis of the studied drugs in their laboratory-prepared mixtures, single tablets and co-formulated tablets. Moreover, the method was applied to an in vitro drug release (dissolution) test. The method was further extended to the determination of LOS in spiked human plasma. Statistical evaluation and comparison of data obtained using the proposed and comparison methods revealed no significant difference between the two methods in addition to good accuracy and precision for the proposed method.

Stability indicating eco-friendly quantitation of terbutaline and its pro-drug bambuterol using quantitative proton nuclear magnetic spectroscopy.

Quantitative 1H-NMR became an increasingly important issue in pharmaceutical analytical chemistry. This study used NMR spectroscopy to assay the bronchodilator drug terbutaline sulfate and its pro-drug bambuterol hydrochloride in pure form and pharmaceutical preparations. The technique proceeded using deuterium oxide (D2O) as an 1H-NMR solvent and phloroglucinol anhydrous as an internal standard (IS). Comparatively, to the phloroglucinol signal at 5.9 ppm, the resulting quantitative signals of the studied drugs were corrected. The terbutaline singlet signal at 6.3 ppm was chosen for quantification, while the bambuterol quantitative singlet signal was at 2.9 ppm. The two drugs were rectilinear over the concentration range of 1.0-16.0 mg/mL. LOD values were 0.19 and 0.21 mg/mL while LOQ values were 0.58 and 0.64 mg/mL for terbutaline and bambuterol respectively. The developed method has been validated according to the International Conference of Harmonization (ICH) regarding linearity, accuracy, precision, specificity, and robustness. A greenness profile assessment was applied, and the method proved to be green. The method enables the assay of the two drugs in pure drug and pharmaceutical preparations. The method also enables the assay of the two drugs in the presence of each other; thus, it is considered a stability-indicating method where terbutaline is an acid degradation product of bambuterol.

Stability-indicating spectrofluorimetric method for determination of itopride hydrochloride in raw material and pharmaceutical formulations.

A simple, sensitive and rapid spectrofluorimetric method for determination of itopride hydrochloride in raw material and tablets has been developed. The proposed method is based on the measurement of the native fluorescence of the drug in water at 363 nm after excitation at 255 nm. The relative fluorescence intensity-concentration plot was rectilinear over the range of 0.1-2 µg/mL (2.5 × 10(-7)-5.06 × 10(-6) mole/L), with good correlation (r = 0.9999), limit of detection of 0.015 µg/mL and a lower limit of quantification of 0.045 µg/mL. The described method was successfully applied for the determination of itopride hydrochloride in its commercial tablets with average percentage recovery of 100.11 ± 0.32 without interference from common excipients. Additionally, the proposed method can be applied for determination of itopride in combined tablets with rabeprazole or pantoprazole without prior separation. The method was extended to stability study of itopride. The drug was exposed to acidic, alkaline, oxidative and photolytic degradation according to ICH guidelines. Moreover, the method was utilized to investigate the kinetics of the alkaline, acidic and oxidative degradation of the drug. A proposal for the degradation pathways was postulated.

Simultaneous determination of floctafenine and its hydrolytic degradation product floctafenic acid using micellar liquid chromatography with applications to tablets and human plasma.

A stability-indicating micellar liquid chromatography (MLC) method was developed and validated for the assay of floctafenine (FLF) in the presence of its degradation product and main metabolite, floctafenic acid (FLA). The analysis was carried out on a CLC Shim-Pack octyl silane (C8) column (150 x 4.6 mm id, 5 microm particle size) using a micellar mobile phase consisting of 0.15 M sodium dodecyl sulfate, 10% n-propanol, and 0.3% triethylamine in 0.02 M orthophosphoric acid (pH = 3). The mobile phase was pumped at a flow rate of 1.0 mL/min with UV detection at 360 nm. The method showed good linearity for FLF and FLA over the concentration ranges of 0.5-25.0 and 0.4-10.0 microg/mL, with LODs of 0.16 and 0.12 microg/mL, respectively. The developed method was successfully applied to the determination of FLF in commercial dispersible tablets, with mean recovery of 98.87 +/- 1.37%. Also, the proposed method was specific for the analysis of FLF in presence of the co-formulated drug thiocolchicoside in laboratory-prepared tablets, with mean recovery of 100.50 +/- 1.07%. Statistical comparison of the results obtained by the proposed MLC method with those obtained by a comparison method showed good agreement. Moreover, the method was extended to study the degradation behavior of FLF under different International Conference on Harmonization recommended conditions such as alkaline, acidic, oxidative, thermal, and photolytic. The method was further applied for direct determination of FLA as the main metabolite of FLF in human plasma without prior extraction steps, with mean recovery of 110.50 +/- 6.5%.

Red cell distribution width, neutrophil lymphocyte ratio and interleukin 10 are good prognostic markers in multiple myeloma.

Background: Multiple myeloma (MM) is still an incurable disease so we need to continue developing new diagnostic and prognostic options for its management. There are multiple prognostic factors for MM, but most of them are costly and time consuming. Hence comes the urge to identify bed side and low cost prognostic tools, that is why this study was aiming to identify in Egyptian MM patients. Materials and methods: The study was carried on 60 newly diagnosed multiple myeloma patients and 20 age and sex matched healthy individuals as controls. Studied subjects were subdivided into two groups: Group I: 60 multiple myeloma patients which were subdivided into three subgroups: Stage I: 10 patients, Stage II: 17 patients, Stage III: 33 patients, Group II: 20 healthy controls. Results: A progressive significant increase in IL-10, RDW, NLR, and beta2 microglobulin (ß2M) with disease progression from stage I towards stage III as compared to the control group. However, IL-10, RDW, and NLR have the best prognostic efficiency value regarding to sensitivity, specificity and positive predictive value when compared with ß2M. Conclusions: IL-10, RDW, and NLR are simple, easy and bedside tests (in the case of RDW, and NLR). They have high sensitivity and specificity when compared to ß2M, which is a well-established prognostic factor that highlights the valuable role they play as prognostic markers in MM.

Fast one-pot microwave-assisted green synthesis of highly fluorescent plant-inspired S,N-self-doped carbon quantum dots as a sensitive probe for the antiviral drug nitazoxanide and hemoglobin.

In this study, we report a one-pot, green, cost-efficient, and fast synthesis of plant-based sulfur and nitrogen self-co-doped carbon quantum dots (S,N-CQDs). By 4-min microwave treatment of onion and cabbage juices as renewable, cheap, and green carbon sources and self-passivation agents, blue emissive S,N-CQDs have been synthesized (λex/λem of 340/418 nm) with a fluorescence quantum yield of 15.2%. A full characterization of the natural biomass-derived quantum dots proved the self-doping with nitrogen and sulfur. The S,N-CQDs showed high efficiency as a fluorescence probe for sensitive determination of nitazoxanide (NTZ), that recently found wide applicability as a repurposed drug for COVID-19, over the concentration range of 0.25-50.0 µM with LOD of 0.07 µM. The nanoprobe has been successfully applied for NTZ determination in pharmaceutical samples with excellent % recovery of 98.14 ± 0.42. Furthermore, the S,N-CQDs proved excellent performance as a sensitive fluorescence nanoprobe for determination of hemoglobin (Hb) over the concentration range of 36.3-907.5 nM with a minimum detectability of 10.30 nM. The probe has been applied for the determination of Hb in blood samples showing excellent agreement with the results documented by a medical laboratory. The greenness of the developed probe has been positively investigated by different greenness metrics and software. The green character of the proposed analytical methods originates from the synthesis of S,N-CQDs from sustainable, widely available, and cheap plants via low energy/low cost microwave-assisted technique. Omission of organic solvents and harsh chemicals beside dependence on mix-and-read analytical approach corroborate the method greenness. The obtained results demonstrated the substantial potential of the synthesized green, safe, cheap, and sustainable S,N-CQDs for pharmaceutical and biological applications.

Eco-friendly spectrophotometric methods for determination of remdesivir and favipiravir; the recently approved antivirals for COVID-19 treatment.

Remdesivir (REM) and Favipiravir (FAV) are recently approved antivirals prescribed in severely ill COVID-19 patients. Therefore, development of new, simple, rapid, sensitive, and selective methods for analysis of such drugs in their pharmaceutical formulations will be highly advantageous. Herein, we have developed different spectrophotometric methods for analysis of the studied analytes. Method I is based on direct spectrophotometric analysis of REM and FAV in ethanol at λmax 244 and 323 nm, respectively. For simultaneous quantitation of REM and FAV, methods II-V were followed. Method II is based on derivative spectrophotometry in which REM was determined in second-order derivative spectra at 248 nm (the zero-crossing wavelength for FAV), while FAV was measured in first-order derivative spectra at 337 nm (the zero-crossing point for REM). Method III is the dual-wavelength method in which spectral intensities were subtracted at 244-207 nm for REM and at 330-400 nm for FAV. Method IV is the ratio subtraction in which ratio spectra were obtained by a suitable divisor followed by subtraction of intensities at 272-340 nm and 335-222 nm for REM and FAV, respectively. Method V is the derivative ratio method in which the obtained ratio spectra in method IV were converted to first-order derivative and then REM and FAV were recorded at 280 and 340 nm, respectively. Calibration graphs were linear in the ranges of 1-10 µg/mL for REM through all methods and 1-20 µg/mL for FAV in methods I and II, and 2-20 µg/mL by the other methods. The evolved methods were applied to pharmaceutical dosage forms of REM and FAV. All the proposed methods were further applied to human plasma samples containing both drugs with acceptable mean recoveries.

Comparative Assessment of SSR and RAPD markers for genetic diversity in some Mango cultivars.

Genetic improvement mainly depends on the level of genetic variability present in the population, and the degree of genetic diversity in a population largely determines the rate of genetic advancement. For analyzing genetic diversity and determining cultivar identities, a molecular marker is a useful tool. Using 30 SSR (simple sequence repeat) and 30 RAPD (randomly amplified polymorphic DNA) markers, this study evaluated the genetic divergence of 17 mango cultivars. The effectiveness of the two marker systems was evaluated using their genetic diversity characteristics. Additionally, the effects of SM (simple matching) and Dice similarity coefficients and their effects on mango clustering were evaluated. The findings showed that SSR markers generated 192 alleles, all of which were polymorphic (100%). With RAPD markers, 434 bands were obtained, 361 of which were polymorphic (83%). The average polymorphic information content (PIC) for RAPD and SSR was 0.378 and 0.735, respectively. Using SSR markers resulted in much higher values for other genetic diversity parameters compared to RAPD markers. Furthermore, grouping the genotypes according to the two similarity coefficients without detailed consideration of these coefficients could not influence the study results. The RAPD markers OPA_01, OPM_12 followed by OPO_12 and SSR markers MIAC_4, MIAC_5 followed by mMiCIR_21 were the most informative in terms of describing genetic variability among the cultivars under study; they can be used in further investigations such as genetic mapping or marker-assisted selection. Overall, 'Zebda' cultivar was the most diverse of the studied cultivars.

Utility and greenness appraisal of nuclear magnetic resonance for sustainable simultaneous determination of three 1,4-benzodiazepines and their main impurity 2-amino-5-chlorobenzophenone.

A robust, stability-indicating, and eco-friendly proton nuclear magnetic resonance (1H-qNMR) method was developed for the concurrent determination of three 1,4-benzodiazepines (BDZs), namely diazepam (DZP), alprazolam (ALP), and chlordiazepoxide (CDP) and their common impurity, synthesis precursor, and degradation product; 2-amino-5-chlorobenzophenone (ACB). In the present method, a novel approach was developed for composing a green and cost-efficient solvent system as an alternative to the common NMR organic solvents utilizing 0.3 M sodium dodecyl sulfate prepared in deuterated water. The conducted method is characterized by simplicity with no need for sample pretreatment or labeling. Phloroglucinol was used as an internal standard. The chosen signals for the determinations of ALP, CDP, DZP and ACB were at 2.35 ppm (singlet), 2.84 ppm (singlet), 3.11 ppm (singlet), and 6.90 ppm (doublet of doublet), respectively. The proposed method possessed linearity over the concentration range of 0.25-15.0 mg ml-1 for DZP, ALP, CDP and of 0.5-25.0 mg ml-1 for ACB with LOD values of 0.06, 0.03, 0.07 and 0.16 mg ml-1 respectively, and LOQ values of 0.18, 0.09, 0.21 and 0.49 mg ml-1, respectively. Accuracy of the method was evidenced by excellent recovery% (99.57-99.90%) and small standard deviation (≥ 1.10) for the three analyzed drugs. Intra- and inter-day precision were determined with coefficient of variation ranging from 0.12 to 1.14 and from 0.72 to 1.67, respectively. For the studied compounds, appraisal of the method greenness was achieved via four approaches: Analytical Eco-Scale, Green Analytical Procedure Index (GAPI), Analytical greenness metric (AGREE), and RGB Additive Color Model. The results proved that the proposed method has the privilege of being a green analytical method.

Validated spectroflurimetric determination of some H1 receptor antagonist drugs in pharmaceutical preparations through charge transfer complexation.

A validated simple, rapid, and selective spectrofluorimetric method was developed for the determination of some antihistaminic H(1) receptor antagonist drugs namely ebastine (EBS), cetirizine dihydrochloride (CTZ), and fexofenadine hydrochloride (FXD). The method is based on the reaction of the cited drugs with some Π acceptors namely p-chloranilic acid (CLA), tetracyanoethylene (TCNE), and 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) to give highly fluorescent derivatives. The fluorescence intensity-concentration plots were rectilinear over the concentration ranges of 0.2-3.0, 0.2-2.5 and 0.15-2.0 µg/ml for EBS with CLA, DDQ, and TCNE respectively; 0.5-7.0, 0.5-6.0, and 0.2-4.0 µg/ml for CTZ with the previously mentioned reagents, and 0.2-3.5, 0.5-6.0, and 0.2-3.5 µg/ml for FXD. The factors affecting the formation of the reaction products were carefully studied and optimized. The method was applied for the determination of the studied drugs in their dosage forms. The results obtained were in good agreement with those obtained by the comparison methods. Reactions Stoichiometries of the complexes formed between the studied drugs and Π acceptors were defined by the Job's method of the continuous variation and found in 1:1 in all cases.

Assessment of leukemia inhibitory factor and glycoprotein 130 expression in endometrium and uterine flushing: a possible diagnostic tool for impaired fertility.

BACKGROUND: Uterine receptivity and implantation are complex processes requiring coordinated expression of molecules by zygote and uterus. Our objective was to evaluate the role of the endometrial expression of leukemia inhibitory factor (LIF) and its glycoprotein 130 (gp130) receptor molecules and their secretion in uterine flushing during the window of implantation in cases of primary unexplained infertility CASE PRESENTATION: The study was conducted on 25 infertile women with unexplained infertility for at least two years and 10 normal fertile women as a control group . Endometrial tissue and uterine flushing were obtained. Each tissue specimen was divided into two pieces; one piece was used for histological dating of the endometrium and for immunostaining of progesterone receptors, and the second was used for RNA extraction and PCR assay of LIF and gp130 mRNA expression. Serum estrogen and progesterone were measured for all subjects. LIF mRNA was expressed in the endometrium of all normal fertile women but significantly decreased in infertile women. LIF was not detectable in 88% of infertile women while it was fairly detectable in 12% of them. Gp130 mRNA was hardly detectable in both fertile and infertile women with no difference between them. Infertile women secreted significantly less LIF and gp130 molecules in the uterine flushing compared with normal fertile women. CONCLUSIONS: Expression of LIF mRNA in endometrium could be used as a molecular marker of unexplained infertility. Assessment of secreted LIF and gp130 molecules in uterine flushing could be another useful and safe method for predicting successful implantation as well as for diagnosing and eventually treating women with impaired fertility using recombinant human LIF.

Development of three ecological spectroscopic methods for analysis of betrixaban either alone or in mixture with lercanidipine: greenness assessment.

Three eco-friendly spectrophotometric methods were developed for determination of the novel anticoagulant drug, betrixaban (BTX). The first method (method A) was based on direct analysis of BTX at 229.4 nm on the zero-order spectrum using methanol as the optimum solvent. While the second method (method B) was based on measuring difference absorption value (ΔA) of BTX at 335 nm, which was obtained from pH-induced spectral difference (difference spectra of BTX in 0.1 M NaOH versus 0.1 M HCl). The third method (method C) was based on measurement of the first-derivative amplitudes of BTX and its co-administered Ca channel blocker lercanidipine (LER) at 304 and 229 nm for simultaneous assay of BTX and LER, respectively. All methods were linear over concentration ranges of 1.0-20.0 and 8.0-80.0 µg ml-1 for BTX in methods A and B, respectively, and of 1.0-20.0 and 1.0-25.0 µg ml-1 for BTX and LER, respectively, in method C. The three methods were fully validated and assessed for greenness by three metrics: analytical eco-scale, green analytical procedure index and Analytical GREEnness metrics. The results indicated the validity and greenness of the proposed methods. Moreover, the methods were applied to assay the studied analytes in their dosage forms with high percentage of recovery and low percentage of relative s.d. values.

Conventional and synchronous spectrofluorometric determination of the recently administered drugs for treatment of COVID-19 favipiravir and apixaban.

COVID-19 is a fast-spreading pandemic that is caused by SARS-CoV-2 viral pathogen. Combination therapy of the antiviral favipiravir and the anticoagulant apixaban is one of the efficient treatment regimens. Therefore, development of novel and sensitive methods for simultaneous analysis of such combination is highly advantageous. Herein, two eco-friendly, simple, rapid, and cost-effective spectrofluorometric methods were evolved for the estimation of favipiravir and apixaban in pharmaceutical and biological matrices. Method I was based on analysis of favipiravir and apixaban by the first-order derivative of the conventional fluorescence spectra obtained after excitation at 300 nm, where favipiravir and apixaban were detected at 468.8 and 432.0 nm, respectively. Method II relied on dual scan synchronous spectrofluorometry, in which favipiravir was determined at 364 nm using Δλ = 60 nm while apixaban was analyzed at 274 nm using Δλ = 200 nm. Method optimization was performed for selecting the optimum conditions at which maximum sensitivity and selectivity were obtained. This report is the first one that describes simultaneous analysis of favipiravir and apixaban by synchronous spectrofluorometry. The developed methods were successfully applied to evaluate favipiravir and apixaban in spiked human plasma and in pharmaceutical dosages with high %recoveries and low RSD.

Utilization of a micellar matrix for simultaneous spectrofluorimetric estimation of alfuzosin hydrochloride and vardenafil hydrochloride.

A sensitive and direct spectrofluorimetric method was developed for simultaneous quantitation of two co-administered drugs, namely, alfuzosin hydrochloride (AFH) and vardenafil hydrochloride (VRH). Both drugs exhibited native fluorescence properties that could be exploited to assay them in biological fluids with high sensitivity. Spectrofluorimetric analysis of AFH and VRH is based on excitation of both drugs at 265 nm where emission spectra were recorded separately for AFH and VRH at 380 and 485 nm, respectively. Micellar trends in analytical chemistry were adopted to minimize both environmental and occupational hazards, using distilled water and sodium dodecyl sulphate (serves as a micellar medium that enhanced the sensitivity of AFH and VRH) for analysis of both drugs in their raw materials, tablets, and human biological fluids (plasma and urine). Linearity ranges were 1.0-16.0 and 10.0-700.0 ng mL-1 for AFH and VRH, respectively. The proposed method was successfully assessed for analysis of AFH and VRH in spiked human plasma and urine samples over the following concentrations: 1.0-12.0 ng mL-1 and 4.0-400.0 ng mL-1 for both drugs, simultaneously with mean recoveries of 101.08 % and 102.06 % in plasma and 96.75 % and 92.8 % in urine. Statistical analysis of the practical results has proved quite good agreement and revealed there were no significant differences in the accuracy and precision with those obtained by the comparison methods. The proposed method was applied successfully to Prostetrol® and Powerecta® commercial tablets without interference with tablet additives.

A synchronous spectrofluorometric technique for simultaneous detection of alfuzosin and tadalafil: applied to tablets and spiked biological samples.

A facile, accurate, eco-friendly and sensitive spectrofluorometric method was evolved to assay alfuzosin hydrochloride (AFH) and tadalafil (TDF) in different matrices. Such a co-administered combination is clinically used for the treatment of lower urinary tract symptoms. Both compounds are characterized by their native fluorescence spectra upon excitation at specific wavelengths. Their characteristic fluorescence spectra were used for sensitive assay of the studied analytes in tablets and human biological samples. The assay principle is based on first-order synchronous spectrofluorometric scan using Δλ = 60 nm in which AFH peaks were recorded at 366 nm. Meanwhile, TDF measurements were recorded at 293 nm in the same scans without overlap with AFH spectra. Recent analytical chemistry trends were implemented to lessen occupational and environmental perils, using ethanol as a diluting solvent for method optimization and application. Linearity ranges were 5.0-90.0 and 10.0-100.0 ng ml-1 for AFH and TDF, respectively in their raw materials with average % recoveries of 100.44% and 99.73% in raw materials, 100.15% and 100.20% in spiked plasma, and 97.14% and 99.99% in spiked urine. The proposed method was successfully applied to Prostetrol and Starkoprex commercial tablets with no interference with common tablet additives.

MiR-150 Expression in Chronic Myeloid Leukemia: Relation to Imatinib Response.

OBJECTIVE: To assess the circulating micro-RNA-150 (miR-150) expression in patients with chronic myeloid leukemia (CML) in relation to imatinib response. METHODS: Sixty patients with CML and 20 age- and sex-matched control subjects were enrolled. Circulating miR-150 levels were assessed by quantitative real-time polymerase chain reaction on days 0, 14, and 90 of imatinib therapy for patients and once for control subjects. RESULTS: The baseline miR-150 expression was significantly lower in patients with CML than in control subjects with subsequent elevation at 14 and 90 days after the start of imatinib treatment. Early treatment response (ETR) at 90 days was the main study outcome. The miR-150 expression had a significantly higher level in patients with CML with ETR. On multivariate analysis, miR-150 on day 14 was significantly related to ETR in patients with CML with predictive efficacy (area under the curve = 0.838, 72.9% sensitivity, and 84.2% specificity). CONCLUSION: We found that miR-150 expression on day 14 of imatinib treatment is a useful early predictive candidate for imatinib response in patients with CML.