Spectrofluorimetric Method Research Articles

Environmentally benign first derivative synchronous spectrofluorimetry for the analysis of two binary mixtures containing duloxetine with avanafil or tadalafil in spiked plasma samples.

Antidepressants can cause sexual dysfunction side effects, necessitating the co-administration of phosphodiesterase type 5 inhibitors. The simultaneous determination of these drugs in biological fluids is critical for therapeutic drug monitoring. For the first time, two binary mixtures containing duloxetine with either avanafil or tadalafil were estimated utilizing simple green spectrofluorimetric methods without the need for a previous separation step. The study was based on first derivative synchronous spectrofluorimetry in ethanol using a change in wavelength difference (∆λ) of 20 and 25 nm for the first and second combinations, respectively. Duloxetine and avanafil were estimated at 297.7 and 331 nm in their binary mixture, while duloxetine and tadalafil were determined at 290.3 and 297.7nm, respectively. The linearity was achieved over the ranges of 0.1-1.5μg mL-1 for both duloxetine and avanafil and 0.01-0.40 μg mL-1 for tadalafil, with limits of detection of 0.013, 0.022, and 0.004 μg mL-1 for duloxetine, avanafil, and tadalafil, respectively. Successful application of the developed approaches was accomplished for the estimation of the two mixtures in dosage forms as well as human plasma with excellent percentage recoveries (96-103.75% in plasma), which supports their suitability for use in quality control laboratories and pharmacokinetic studies. Moreover, the adopted approaches' greenness was evidenced by applying three tools.

A novel optimized eco-friendly simple spectrofluorimetric method for the determination of total catechins in green tea extract: Application to commercial tablet.

Green tea extract (GTE) contains antioxidants that are present in green tea. The active constituents of green tea extract are catechins. This study demonstrates a spectrofluorimetric method for measuring GTE's catechin concentration based on its native fluorescence. To design a quick, sensitive, and ecological spectrofluorimetric approach, all features were investigated and adjusted. This method relies on determining the GTE ethanolic solution's native fluorescence at 312 nm after excitation at 227 nm. The calibration graph displayed a linear regression for values between 0.05 and 1.0μg mL-1. The detection and quantification limits of the proposed technique were 0.008 and 0.026 μg mL-1, respectively. Two pure catechins present in GTE, (-)-epicatechin and (-)-epigallocatechin gallate, were examined by the proposed method. The analytical estimation of GTE in the pharmaceutical tablet was achieved effectively using this approach. An adequate degree of agreement was found when the findings were compared to those obtained by the comparative technique. Therefore, the novel strategy may be used in the GTE quality control study with minimal risks to people or the environment. The quantum yields of catechins were estimated. The validated technique was accepted by the International Council of Harmonization criteria.

Two green and sensitive spectrofluorimetric approaches for determination of Ambroxol and guaifenesin in their single and combined pharmaceutical formulations.

Ambroxol hydrochloride (AMX) and guaifenesin (GFN) are approved drugs utilized to treat coughs through their potent mucolytic and expectorant properties. Due to their massive, combined administration in many illnesses, there is a persistent need for their concurrent estimation in different pharmaceutical formulations. Two sensitive, environmentally friendly spectrofluorimetric methods were developed. AMX was determined using the first method (I) without interference from GFN. This method depends on the quenching of Erythrosine B (EB) native fluorescence at 552 nm after excitation at 527 nm due to the formation of a non-fluorescent AMX-EB ion-pair complex in Britton-Robinson buffer (BRB) solution pH (3.5). The concentration plot is linear over the 0.25-5.0μg/mL range, with a mean percent found value of 99.74%. Method (II) depends on measuring the native fluorescence of aqueous GFN solution at two analytical wavelengths, either 300 or 600 nm, after excitation at 274 nm. Relative fluorescence intensity (RFI)-concentration plots are linear over the ranges of 0.02-0.5 and 0.1-2.0μg/ml, with mean percent found at 99.96% and 99.91% at dual wavelengths, respectively. The proposed methods were successfully applied to assay both drugs in raw materials and different single and combined pharmaceutical formulations. These methods have been thoroughly validated following International Committee on Harmonisation (ICH) guidelines. National Environmental Methods Index, Analytical Eco-Scale, and Green Analytical Procedure Index were used to prove greenness, thereby enhancing their applicability. The proposed techniques provide straightforward, precise, and cost-effective solutions for routine formulation analysis in quality control laboratories.

Derivatization-free CTAB-induced fluorescence sensing strategy for determination of daptomycin in environmental, pharmaceutical, and biological samples

A simple, economical, green, and sensitive spectrofluorimetric method was developed for the determination of the cyclic lipopeptide antibiotic daptomycin (DPT). The method is based on the sensitizing effect of the cationic surfactant cetyltrimethylammonium bromide (CTAB) on the weak fluorescent signal of DPT. After excitation at 373 nm, DPT-CTAB fluoresces at a maximum intensity of 458 nm. Under the optimized conditions, the method exhibits linearity over the concentration range of 0.50–10.0 μg/mL with a detection limit down to 0.11 μg/mL. The study revealed excellent selectivity towards DPT in the presence of the co-administered drugs. The proposed method was able to determine DPT in its commercial vials, and the results were comparable to those obtained by the reported method. The high sensitivity of the developed method allowed its estimation in water and biological fluids (spiked plasma and urine samples) with high % recoveries (95.89–105.99%). DPT was successfully determined in rat plasma after intra-peritoneal administration, and the method was applied for the calculation of its pharmacokinetic parameters (Cmax, t1/2, tmax, and AUC) in rat plasma. Comparison with the reported methods reveals many benefits of the proposed spectrofluorimetric method, such as greenness, simplicity, sensitivity, and reliability. Finally, different recent assessment tools confirmed the greenness and whiteness of the proposed method.

Spectrofluorimetric determination of butylated hydroxytoluene and butylated hydroxyanisole in their combined formulation: application to butylated hydroxyanisole residual analysis in milk and butter

Butylated hydroxytoluene (BHT) and butylated hydroxyanisole (BHA) are two antioxidants that have been extensively used in many applications. Both are well known for their debatable health risks due to their multiple intake sources. Therefore, conservative limits are set for them in different regulations adapted to the matrices in which they exist. Here we present a simple spectrofluorimetric method for the determination of BHT and BHA based on their native fluorescence and synchronous scanning mode. The type of solvent and the interval between emission and excitation wavelengths were carefully optimized. Under the optimized conditions, good linearities were obtained between the emission intensity and the corresponding concentrations of BHT and BHA over the range of 3–18 µg/mL and 0.1–7 µg/mL, respectively with a good correlation coefficient (r > 0.99). The limits of detection were 0.9 and 0.02 µg/mL, and the quantification limits were 3 and 0.05 µg/mL for BHT and BHA, respectively. The suggested procedure was validated according to ICH guidelines Q2 (R1). Furthermore, the method’s greenness was assessed by three different methods, and it proved to be eco-reasonable. The method was successfully applied to the determination of BHT and BHA in pharmaceutical formulations. We also applied the suggested method for monitoring the residual BHA in conventional, powdered milk and butter, with good recovery in spiked samples.

Utility of green chemistry for sustainable fluorescence derivatization approach for quantification of fingolimod as antineoplastic drug in pharmaceutical formulation and spiked human plasma

Fingolimod is the immune-suppressive medication, that largely used for multiple sclerosis treatment, thought to be the most prevalent inflammatory condition affecting the central nervous system (CNS). Here in, a second spectrofluorimetric method was advanced for quantifying of fingolimod in pharmaceutical formulation and spiked human plasma. That method depends on fluorescence derivatization of fingolimod with 4‑chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) at 75°C in a (pH 9) of borate buffer to produce a fluorescent derivative which can be detected at 540 nm afterwards excitation at 475 nm. The method has been validated using international conference of harmonization (ICH criteria), and it demonstrated linearity in a range of 1–100 ngmL−1. The proposed method was applied precisely and accurately for quantifying fingolimod within pharmaceutical formulation and spiking human plasma without any interferences. The proposed method was more sensitive, about six folds of intensity of the reported spectrofluorometric method and greenness comparison was done only on the proposed method . Moreover, the method's sustainability was evaluated and compared to the published method using two greenness assessment tools termed analytical eco-scale and Analytical GREENness (AGREE). That findings suggest that the method is more sustainable than the published method.

Determination of antihistaminic drugs alcaftadine and olopatadine hydrochloride via ion-pairing with eosin Y as a spectrofluorimetric and spectrophotometric probe: application to dosage forms

Four sensitive and fast analytical approaches relied on ion pairing with eosin Y were built up and evaluated using spectroscopy for determination of Alcaftadine and Olopatadine hydrochloride with high sensitivity and selectivity. Two spectrofluorimetric techniques were employed to observe the quenching effect of Alcaftadine or Olopatadine hydrochloride on the intrinsic fluorescence of eosin Y in a 0.1 M acetate buffer solution at pH 3.8 and 3.3 for Alcaftadine and Olopatadine hydrochloride, respectively. Those methods are considered the first spectrofluorimetric methods for Alcaftadine and Olopatadine hydrochloride assay. The fluorescence quenching effect was linear with concentration ranging from 150 to 2000 and 200 to 2000 ng mL−1 for Alcaftadine and Olopatadine hydrochloride, respectively. In the two spectrophotometric techniques, the absorbance of the produced ion-pair was monitored at 548 and 547 nm in aqueous buffered solution at pH 3.8 and 3.3 for Alcaftadine and Olopatadine hydrochloride, respectively. Beer's law was obeyed in the concentrations range of 0.8–8.0 and 1.0–10.0 µg mL−1. The four techniques were evaluated in accordance with ICH requirements and were effectively used to analyze dosage forms with a high percent recovery.

Comprehensive strategy of white analytical chemistry and analytical quality by design to sensitive spectrofluorimetric method for in-vitro drug release kinetic study of Ibrutinib-loaded nanostructured lipid carriers for leukemia via lymphatic targeting

Ibrutinib (IBR) is a drug classified as BCS class II, characterized by low solubility and high permeability. However, its oral bioavailability is limited to a mere 2.9% due to significant first-pass metabolism. To address this challenge, researchers developed IBR-NLCs (Nanostructured Lipid Carriers) using a DoE-based hot melted ultrasonication method to enhance its bioavailability and drug release profile. While various methods exist for IBR analysis in pharmaceutical formulations, human plasma, and rat plasma, a sensitive spectrofluorimetric method has not been reported for estimating IBR. To facilitate in-vitro drug release kinetic studies of IBR-NLCs, a sensitive and green spectrofluorimetric method was developed, combining principles of white analytical chemistry and analytical quality by design. This approach included a fractional factorial design for screening of method variables and a Box-Behnken design for method optimization. The developed method underwent rigorous validation following ICH guidelines. The developed method was applied to assess the in-vitro drug release kinetic study of IBR-NLCs in comparison to marketed formulations. Remarkably, the optimized IBR-NLCs exhibited sustained release of IBR which helps to decrease dose and dose frequency. The whiteness and greenness profiles of published and proposed method have been assessed using analytical greenness calculator, green analytical procedure index software, national environmental method index standards, and eco-scale assessment tool. The results confirmed that the proposed method is sensitive, eco-friendly, cost-effective, speedy, and user-friendly, making it an excellent choice for IBR estimation in NLCs. In summary, the developed method for drug release kinetic study of BR-NLCs, utilizing principles of white analytical chemistry and analytical quality by design, has not only improved drug release profile but also resulted in an efficient and environmentally friendly analytical approach.

A Novel Spectrofluorimetric Determination of Antazoline and Xylometazoline in their Ophthalmic Formulation; Green Approach and Evaluation.

A green developed spectrofluorimetric method has been applied for Antazoline (ANT) and Xylometazoline (XLO) determination in both pharmaceutical formulation and pure form. The developed method is synchronous spectrofluorimetry coupled with the second derivative mathematical tool for the determination of antazoline and xylometazoline in their dosage form. The developed method depends on reacting the cited drugs with dansyl chloride, a suitable derivatizing agent, to generate highly fluorescent derivatives. The products formed were measured at emission wavelengths; 703.0 and 712.0nm after being excited at wavelengths; 350.0 and 355.0nm for antazoline and xylometazoline, respectively. Synchronous spectrofluorimetry coupled with second derivative mathematical tool was developed and optimized using fluorescence data manager software generating second derivative peak amplitudes at 556.5nm for antazoline and 598.0nm for xylometazoline. Linear responses have been represented over a wide range of concentration 0.5-12.0µg/mL for antazoline and 0.1-10.0µg/mL for xylometazoline, correspondingly. Method validation was successfully applied. Additionally, statistical comparison of developed method with official ones has been carried out where no significant difference was found. Evaluation of the method's greenness was proven using several assessment tools. Indeed, the method developed is found to be precise, sensitive, and discriminating to assess the cited drugs for regular analysis.

Eco-friendly, sensitive and inventive first derivative synchronous spectrofluorimetric determination of ciprofloxacin and phenylephrine in their pure form, single and combined eye drops

A facile, sensitive, accurate and green spectrofluorimetric method was evolved for the assay of ciprofloxacin hydrochloride (CFX) and phenylephrine hydrochloride (PLN) in their co-formulated eye drops with their challengeable ratio of 30:1 for CFX and PLN, respectively. Such drops are clinically used for the treatment of eye bacterial infections. They relieve the symptoms of infection by stopping further growth of the causative microorganisms. The assay principle based on first-order synchronous spectrofluorometric scan using Δ λ = 40 nm in which PLN peak amplitudes were recorded at 283.4 nm, meanwhile CFX was measured at 326.2 nm in the same scans. The calibration curves were linear within the concentration ranges: 0.02–0.5 µg/mL and 0.5–5.0 µg/mL for PLN and CFX, respectively. The method validation was confirmed following the International Conference of Harmonization (ICH) Guidelines. This suggested method was the first one that described simultaneous analysis of PLN and CFX by a spectrofluorimetric technique. In this method, green analytical procedures were implemented to lessen occupational and environmental perils and method greenness was assessed by four assessment tools. GAPI, NEMI, AGREE and Analytical eco-scale were applied to this study and it was deduced from their results that the method had high degree of greenness as it fulfilled all requirements of GAPI, NEMI pictograms and it had high scores of analytical eco scale (97) and AGREE methods (0.82). Subsequently, it was successfully applied to assay both drugs in pure forms, pharmaceutical single and co-formulated eye drops.

Extraction-less green spectrofluorimetric method for determination of mercury using an Astra Phloxine fluorophore: Comprehensive experimental and theoretical studies

A new sensitive and selective extraction-less method for the spectrofluorimetric determination of Hg2+ has been developed using the polymethine dye Astra Phloxine (AP) with requirements for green analytical chemistry. The principle of this method for analytical use is the formation of an ion associate (IA) in the presence of mercury ions and AP, which causes a change in the electronic structure of the dye cation and its subsequent fluorescence quenching. The IA created during the process was sufficiently stable in aqueous solutions and did not require the use of surfactants or organic solvents, which are typically used for similar analytical systems. The system indicated high selectivity towards Hg2+ in the presence of at least 100-fold higher concentrations of Co2+, Fe2+, Mg2+, Ni2+, Zn2+, Ca2+, Ba2+, K+, Na+. The calibration curve was linear in the range from 0.003 to 0.1 mg L–1. Precision and accuracy were expressed as intra-day and inter-day analysis with RSD values of 2.9 – 4.8 % and recovery of 97.1 – 110.0 %. The proposed method was used for the determination of Hg2+ on the model and real water samples. Theoretical calculations were used to predict the IA structure and to explain the experimentally observed fluorescence spectra. A few theoretical methods were tested for predicting IA emission energies, and the CIS(D) method was found to be the most accurate.

Coordination polymer gel mediated spectrophotometric, ICP-AES and spectrofluorimetric methods for trace As(III) determination in water and food samples

Herein, a coordination polymer gel is proposed for the determination of As(III) in real samples through multispectroscopic techniques viz. spectrophotometry, spectrofluorimetry, and inductively coupled plasma atomic emission spectroscopy (ICP-AES). Taguchi L32 (46 21) design and adaptive neuro fuzzy inference system (ANFIS) optimized the controllable factors affecting the extraction yielding an experimental S/N ratio of 39.94 dB. The fluorescence quenching (KSV = 2.63 × 106 L mol−1) was static with photoelectron transfer being the main mechanism confirmed by the density functional theory calculations. The limits of detection (LODs), limits of quantification (LOQs) and linear ranges were 0.038 μg L−1, 0.13 μg L−1 and 1.67–116.67 μg L−1, 0.40 μg L−1, 1.21 μg L−1 and 1.67–33.33 μg L−1, 1.07 μg L−1, 3.24 μg L−1 and 3.32–35.37 μg L−1 for the developed enrichment coupled ICP-AES, spectrophotometry and fluorescence sensing methods. Among these methods, the enrichment - ICP-AES method has the lowest LOD, LOQ and the widest linear range followed by the enrichment - spectrophotometry and fluorescene sensing methods. Spectrofluorimetry offers high sensitivity, selectivity, and possible real time monitoring, spectrophotometry provides a cost-effective and versatile option, while ICP-AES manifests multi-element analysis with high sensitivity and low interference. The developed methods were validated and employed for the successful determination of trace As(III) in real samples. The employment of these methods enhances the overall analytical capability for a wide range of sample types and concentrations.

Integration of sustainable chemistry frameworks with a single-pot, on-off fluorescence approach for enabling the facile quantification of mosapride; Application to pharmaceutical tablets and content uniformity

The twelve green chemistry concepts were considered for designing two new feasible, sensitive and selective spectroscopic approaches for the estimation of mosapride (MSP) in pure powder and tablet dosages. These approaches were derived from the reaction of the drug with erythrosine B in buffered acidic medium. The reaction yielded a binary complex, and its absorbance can be measured at its λmax (556 nm) while the incorporation of erythrosine B in the complexation reaction caused quantitative quenching of its native fluorescence that could be measured at 554 nm after excitation at 529 nm. The reaction parameters were carefully optimized for the two methods then the calibration curves were plotted. The absorbance and fluorescence quenching were directly proportional to MSP concentration in the ranges of 1.0–12.0 and 0.15–2.0 μg/mL, respectively. Limits of detection and quantitation were estimated giving values of 0.30 and 0.92 μg/mL for spectrophotometric method and 0.047 and 0.143 μg/mL for spectrofluorimetric method. In accordance with the International Council for Harmonization (ICH) guiding rules, the new methods were assessed proving their high accuracy, precision, and robustness. The methods were adopted for the determination of the cited drug in pharmaceutical tablets. Moreover, the uniformity of tablet contents was successfully tested according to USP utilizing the suggested approaches. Furthermore, the greenness of the suggested procedure was confirmed using three different approaches.

Обзор спектрофлуориметрических исследований кожных покровов

Background. Nicotinamide adenine dinucleotide (NADN) is involved in many important biochemical reactions in human metabolism, including participation in mitochondrial energy production. Mitochondrial activity, which affects skin microcirculation and the efficiency of local blood supply, can be indirectly assessed by the fluorescence of NADH in its reduced form. Changes in major skin fluorophores have been studied in both animals and humans, at rest and under different conditions, using spectrofluorimetry. The purpose of the work is, based on scientific literature data, to evaluate the possibility of using a spectrofluorimetric study of NADH levels, as well as the NADH/FAD ratio when assessing the condition of both free skin flaps and pedicled flaps after reconstructive operations, in particular in ophthalmology. Materials and methods. A search of scientific publications in PubMed, Google Scolar and Elibrary was conducted, as a result 61 articles for the period of 1957-2022 were selected for the final scientific review. Results and discussion. A brief historical background of the first spectrofluorimetric studies is presented. A brief overview of spectrofluorimetric methods for studying the skin of both humans and experimental animals, as well as other organs and systems, is given. The disadvantages and advantages of various research methods are listed. A review of changes in spectrofluorimetric parameters of the skin in patients with various somatic diseases of organs and systems was carried out. Conclusion. A review of the abovementioned methods for assessing tissue metabolism is applicable in surgical treatment, plastic surgery and onco-ophthalmology. Of particular value for surgery will be research methods that make it possible to predict the likelihood of rejection of transplanted skin flaps and their cicatricial changes. The presented literature review confirms the effectiveness of spectrofluorimetry for assessing metabolic disorders in the skin. The relevance of the method for predicting cosmetic outcomes during plastic surgery, including on the adnexal apparatus of the eye, requires continued research into the main fluorophores of the skin.

A Novel quality-by-design optimized spectrofluorimetric approach for estimation of the oral synthetic adiponectin receptor agonist AdipoRon in different biological matrices: Compliance with greenness metrics

The current study introduces the first analytical approach for the quantitative analysis of adipoRon, a synthetic adiponectin receptor agonist, using a facile, rapid, sensitive, and green spectrofluorimetric method. Nitrogen-doped carbon quantum dots (N-CQDs) were synthesized by adopting a fast microwave-assisted procedure using accessible and natural substrates (orange juice and urea). The suggested synthetic method produced CQDs with narrow particle size distribution (2–10 nm), high fluorescence stability, and good quantum yield (29.3%). The produced fluorescent QDs were used as fluorescent sensors and were quantitatively quenched by increasing adipoRon concentrations. A two-level full factorial design (22 FFD) was used to identify the most critical experimental factors affecting the relative fluorescence intensity of N-CQDs. The fluorescence quenching of N-CQDs by the drug was measured at 417 nm after excitation at 325 nm. Under the optimized conditions, the quenching of N-CQDs' fluorescent intensity displayed acceptable linearity with the adipoRon concentration range of 5.0–20.0 μg/mL with limits of quantitation and detection of 0.843 μg/mL and 0.278 μg/mL, respectively. Owing to the high sensitivity, the suggested method was efficiently applied for adipoRon estimation in different biological matrices, including spiked human plasma, real rat plasma, and liver homogenate samples with high % recoveries (87.41–103.17%) and low %RSD values (<2.87%). The method's greenness was evaluated using two metric tools, the complementary green analytical procedure index (ComplexGAPI) and the Analytical GREENNESS metric approach (AGREE), and the results showed that the method was excellent green. The proposed methodology was validated according to the ICHQ2 (R1) recommendations.

Ecological assessment and development of analytical methods for concurrent quantification of valsartan and sacubitril: whiteness comparative study based on relative scoring.

Sustainable analytical chemistry is gaining great interest in global environmental pollution control. In addition, valsartan (VAS) and sacubitril (SAB) have been recently approved by the FDA as a fixed-dose combination "LCZ696". It showed efficacy and safety enough to extend its application from heart failure to hypertension control. VAS/SAB dual therapy is considered expensive; however, its prescription has increased significantly worldwide. This prescription increased the demand for developing sustainable analytical methods that simultaneously analyze VAS and SAB. Highly sensitive and selective spectrofluorimetric methods have been developed for this purpose. A synchronous spectrofluorimetric technique was applied. In one method, it was followed by spectral derivatization at the first-order level. The signals were recorded at 230 and 211 nm for VAS and SAB, respectively. Synchronous spectrofluorimetry was coupled to a dual-wavelength mathematical approach in the second method. Signals were derived by subtracting synchronous responses at 241 nm, 226 nm, and 239 nm from the response at 208 nm for VAS and SAB, respectively. Method validation was carried out following ICH guidelines. VAS showed linear calibration curves spanning the range of 60-200 and 80-600 ng mL-1 for the derivative and dual wavelength-assisted approaches, respectively. SAB achieved linear responses in the range of 17-190 and 30-350 ng mL-1 for the first and second methods, respectively. The green profile of the proposed methods was confirmed using the analytical eco-scale (AES), green analytical procedure index (GAPI), and analytical greenness metric (AGREE) tools. The proposed hybrid methods proved highly sustainable through the whiteness RGB 12 algorithm evaluation approach. Whiteness was comparatively assessed for the proposed and reported methods based on relative scoring depending on the parameters of each method. Despite this scoring approach being accurate as a relative score for comparative purposes, it gave rise to underestimated absolute scores. Therefore, to obtain a proper conclusion from the comparative whiteness study, all the methods were ranked according to their whiteness score, illustrating the excellent whiteness ranks of the proposed methods. Upon complete comparison with the reported methods, the suggested ones showed several advantages concerning analytical performance and the greenness level. The proven affordability and simplicity encourage their wide industrial application in developing countries.

Optimization of the Method for Spectrofluorimetric Determination of Aluminum Impurities in Substances

Introduction. Evaluation of the content of impurities is the most important step in confirming the safety and efficacy in the quality control of the medicinal product. Aluminum, being an acceptable impurity in a number of pharmaceutical substances, can adversely affect the human body, as a result of which its content is normalized. The admixture of aluminum in the State Pharmacopoeia of the Russian Federation XV is determined by the spectrofluorimetric method using the ligand – 8-hydroxyquinoline in chloroform. In the present work, it is proposed to replace 8-hydroxyquinoline with the more accessible rutin, which also forms fluorescent complexes with metals. This approach involves the exclusion of the stage of extraction of the aluminum complex into chloroform from sample preparation, which improves the accuracy of the technique, and the replacement of chloroform has a positive effect on safety.Aim. To create an alternative approach for the spectrofluorimetric determination of aluminum impurities using rutin and "potassium chloride" as an active pharmaceutical ingredient.Materials and methods. The following substances and reagents were used as research materials: CRS of aluminum ion 1 mg/ml (LLC "EKROSHIM", Russia), CRS of iron ion (II) 1 mg/ml (LLC "EKROSHIM", Russia), CRS of zinc ion 1 mg/ml (LLC "EKROSHIM", Russia), CRS of lead-ion 1 mg/ml (LLC "EKROSHIM", Russia), CRS nickel-ion 1 mg/ml (LLC "EKROSHIM", Russia), CRS copper-ion 1 mg/ml (LLC "EKROSHIM", Russia), chromium (III) cation standard 1 mg/ml (imp., Sigma-Aldrich, USA) rutin (imp., Sichuan Guangsong Pharmaceutical Co., Ltd., China), ammonium acetic acid (imp., Molekula GmbH, Germany), glacial acetic acid (chemically pure, JSC "Base No. 1 Himreaktivov", Russia), potassium chloride (pharmaceutical substance, LLC "MZHR", Russia). The spectrofluorimetric study was carried out on an FL 6500 instrument (PerkinElmer Inc., USA). The aluminum impurity content was also evaluated using an Optima 8000 inductively coupled plasma atomic emission spectrometer (ICP AES) (PerkinElmer Inc., USA) and a Multi-Element Solution standard sample (PerkinElmer Inc., USA).Results and discussion. The approach given in the article eliminates the use of 8-hydroxyquinoline in chloroform and replaces it with rutin in 70 % ethyl alcohol. The aluminum-rutin complex has an excitation wavelength at 445 nm and an emission wavelength at 565 nm. The proposed method was tested on the substance "Potassium chloride" to assess the indicator "Aluminum", the content of which should not exceed 0.0001 %. Method validation was carried out according to three parameters "Specificity", "Linearity" and "Limit of detection". Comparison of the data obtained was carried out using atomic emission spectroscopy, during which the relevance of the technique was proved.Conclusion. An ergonomic approach has been developed for the spectrofluorimetric determination of aluminum impurities using rutin with approbation on the substance "Potassium chloride". The results obtained during the experiment were confirmed by the ICP AES method.

Total Selenium Level and Its Distribution between Organs in Beef Cattle in Different Selenium Status.

The aim of this study was to determine the Se concentration in the main tissues of beef cattle and to evaluate the differences in tissue distribution between animals with different selenium status. Selenium concentration was determined in the serum, longissimus dorsi muscle, semitendinosus muscle, kidney, heart, liver, spleen and lungs of cows, heifers and beef bulls, using spectrofluorimetric method. Despite receiving supplementation, 55.6% animals demonstrated an optimal Se level, while 44.4% were deficient. The mean serum Se concentration was significantly higher (p < 0.05) in animals with a normal Se status than in Se-deficient animals. Differences in Se tissue distribution were observed between Se-deficient animals and those with normal Se status. The organs most susceptible to Se deficiency are the semitendinosus muscle, lungs, heart and liver. In both normal and Se-deficient animals, significantly higher Se concentrations were observed in the kidney than other organs (p < 0.05), and the lowest in the muscles. As Se deficiencies can be found among supplemented animals, the level of Se should be monitored in beef cattle in order to detect possible Se deficiencies, which may have negative health effects for animals and reduce the value of animal products as a source of Se in the human diet.

Eco‐friendly synchronous fluorescence spectrofluorimetric method for simultaneous determination of montelukast sodium and fexofenadine hydrochloride in their antiallergic rhinitis fixed‐dose combination tablets

AbstractAn innovative, simple, accurate, sensitive, and eco‐friendly synchronous fluorescence spectrofluorimetric method has been developed for the simultaneous analysis of montelukast sodium (MON) and fexofenadine hydrochloride (FEX). The method relies on measuring the relative synchronous fluorescence intensity of both drugs using Δλ of 60 nm in methanol at 405 nm for MON and 288 nm for FEX. The experimental parameters influencing the developed method were investigated and optimized. The method was linear over the ranges 0.1–2.0 and 2.0–20.0 μg/ml for MON and FEX, respectively. The limits of detection were 0.018 and 0.441 μg/ml, and the limits of quantitation were 0.055 and 1.336 μg/ml for MON and FEX, respectively. The developed method was applied successfully for the determination of the two drugs in their newly released fixed‐dose combination prescribed for the treatment of allergic rhinitis. The mean per cent recoveries were found to be 100.680 ± 0.890 and 100.110 ± 0.940 for MON and FEX, respectively. Furthermore, the method was found to be eco‐friendly green as was evaluated according to the Green Analytical Procedure Index tool guidelines and analytical eco‐scale.

Development and validation of synchronous spectrofluorimetric method for the simultaneous determination of duvelisib and moxifloxacin: greenness metric assessment and application to a pharmacokinetic study in rats

Duvelisib (DUV) is a potent anticancer drug whereas Moxifloxacin (MOX) is an antimicrobial drug with anti-proliferative potency against cancerous cells, which is empirically administered in cancer treatment. DUV and MOX combination is commonly prescribed to combat infections in patients while they are under chemotherapy treatment. This study describes, for the first time, the development of a simple and green synchronous spectrofluorimetric (SSF) method for the simultaneous estimation of DUV and MOX in plasma. DUV and MOX were quantified at 273 and 362 nm, respectively without interference between each other at Δλ of 120 nm. The experimental variables influencing fluorescence intensities were thoroughly investigated and the optimum conditions were established. At pH 3.5, the optimum synchronous fluorescence intensity (SFI) was achieved in water solvent by using sodium acetate buffer solution. Calibration curves for DUV and MOX, correlating the SFI with the corresponding drug concentration, were linear in the range of 50–1000 ng mL−1 for both drugs, with good correlation coefficients. The method was extremely sensitive, with limits of detection of 24 and 22 ng mL−1, and limits of quantitation of 40 and 45 ngmL−1 for DUV and MOX, respectively. The SSF method was validated according to the Food and Drug Administration (FDA) guidelines for validation of analytical procedures, and the validation parameters were acceptable. The proposed SSF method was applied to the pharmacokinetic and bioavailability studies in rats’ plasma after single concurrent oral administration of both drugs. The results of the study revealed that caution should be taken with DUV dose when concurrently administered with MOX. The greenness of SSF method was assessed by three different metric tools namely Analytical Eco-scale, Green Analytical Procedure Index, and Analytical Greenness Calculator. The results confirmed that SSF method is an eco-friendly and green analytical approach. In conclusion, the proposed SSF method is a valuable tool for pharmacokinetic/bioavailability studies and therapeutic drug monitoring of simultaneously administered DUV and MOX.