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One of the most common features of many different clinical conditions is pain; hence, there is a crucial need for eliminating or reducing it to a tolerable level to retrieve physical, psychological and social functioning. A first derivative synchronous spectrofluorimetry technique is proposed for the simultaneous determination of celecoxib and tramadol HCl, a recent coformulation authorized for treating acute pain in adults. The method includes using synchronous spectrofluorimetry at ∆λ = 80 nm where tramadol HCl was determined using first derivative technique at λ = 230.2 nm, while celecoxib was determined at λ = 288.24 nm. The proposed method was successfully applied to their co‐formulated dosage forms in addition to spiked human plasma and validated in agreement with the guidelines of the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). The linear ranges were found to be 0.50–5.0 and 0.15–0.50, the limits of detection to be 0.088 and 0.011 and the limits of quantification to be 0.266 and 0.032 μg/ml for celecoxib and tramadol, respectively. Statistical analysis revealed no significant difference when compared with previously reported methods as evidenced by the values of the variance ratio F‐test and Student t‐test. The proposed method was successfully applied to commercial dosage forms and spiked human samples. Moreover, the greenness of the proposed method was investigated based on the analytical eco‐scale approach, with the results showing an excellent green scale with a score of 95. [ABSTRACT FROM AUTHOR]

A meta‐analysis was performed to identify patients with coronavirus disease 2019 (COVID‐19) presenting with gastrointestinal (GI) symptoms during the first and second pandemic waves and investigate their association with the disease outcomes. A systematic search in PubMed, Scopus, Web of Science, ScienceDirect, and EMBASE was performed up to July 25, 2020. The pooled prevalence of the GI presentations was estimated using the random‐effects model. Pairwise comparison for the outcomes was performed according to the GI manifestations' presentation and the pandemic wave of infection. Data were reported as relative risk (RR), or odds ratio and 95% confidence interval. Of 125 articles with 25,252 patients, 20.3% presented with GI manifestations. Anorexia (19.9%), dysgeusia/ageusia (15.4%), diarrhea (13.2%), nausea (10.3%), and hematemesis (9.1%) were the most common. About 26.7% had confirmed positive fecal RNA, with persistent viral shedding for an average time of 19.2 days before being negative. Patients presenting with GI symptoms on admission showed a higher risk of complications, including acute respiratory distress syndrome (RR = 8.16), acute cardiac injury (RR = 5.36), and acute kidney injury (RR = 5.52), intensive care unit (ICU) admission (RR = 2.56), and mortality (RR = 2.01). Although not reach significant levels, subgroup‐analysis revealed that affected cohorts in the first wave had a higher risk of being hospitalized, ventilated, ICU admitted, and expired. This meta‐analysis suggests an association between GI symptoms in COVID‐19 patients and unfavorable outcomes. The analysis also showed improved overall outcomes for COVID‐19 patients during the second wave compared to the first wave of the outbreak. Highlights: •Gastrointestinal (GI) symptoms in COVID‐19 patients were associated with unfavorable outcomes.•Cases presenting with GI symptoms on admission were more subjected to complications.•GI cohorts of COVID‐19 cases showed a double risk of ICU admission and mortality.•Overall outcomes for COVID‐19 patients during the second wave showed improvement compared to the first wave of the outbreak. [ABSTRACT FROM AUTHOR]

Simple and rapid synchronous fluorometric methods were adopted and validated for the simultaneous analysis of a binary mixture of diphenhydramine (DIP) and ibuprofen (IBU) (Mix I) or DIP and phenylephrine (PHE) (Mix II) in their co‐formulated pharmaceuticals without prior separation. Analysis of Mix I is based on the measurement of the peak amplitudes (D1) of synchronous fluorescence intensities at 265.1 nm for DIP and 260 nm for IBU. The relationship between the concentration and the amplitude of the first‐derivative synchronous fluorescence spectra showed good linearity over the concentration ranges 0.50–10.00 μg ml−1 and 0.50–7.90 μg ml−1 for DIP and IBU, respectively. Analysis of Mix II was based on measurement of the peak amplitude (D1) synchronous fluorescence intensities at 230 nm for DIP and at 253.9 nm for PHE. Moreover, for Mix II, the peak amplitude (D2) synchronous fluorescence intensities were measured at 227.9 nm for DIP and at 264.9 nm for PHE. Calibration plots were rectilinear over the concentration range 0.30–3.50 μg ml−1 and 0.03–0.75 μg ml−1 for DIP and PHE, respectively. The proposed methods were successfully applied to determine the studied compounds in pure form and in pharmaceutical preparations. [ABSTRACT FROM AUTHOR]

In this study, two analytical approaches were exploited for the resolution of binary mixtures of ciprofloxacin HCl (CIP) or norfloxacin (NOR) and phenazopyridine HCl (PHZ). In the first approach, the amplitudes of the first derivative of the ratio spectra were measured at 267 or 287 nm for CIP and at 268 or 291 nm for NOR. PHZ could be directly determined in the presence of CIP or NOR at 405 nm. The calibration graphs were rectilinear over the ranges of 1.0-16.0 μg/mL for CIP or NOR and 1.0-10.0 μg/mL for PHZ. In the second approach, an accurate, reliable and environmentally nontoxic micellar liquid chromatographic (MLC) method was developed. A good chromatographic separation was achieved using a 150 mm× 4.6 mm i.d., 5 μm particle size Spherisorb ODS-2 column. Eco-friendly mobile phase containing 0.12 M sodium dodecyl sulphate, 0.3% triethylamine and 6% n-butanol in 0.02 M orthophosphoric acid of pH 3.0 was pumped at a flow rate of 1 mL/min. Time programmed UV-detection was applied to allow sensitive determination of the studied drugs. The analytes were eluted without interferences in <10 min. Methocarbamol was used as an internal standard. The MLC methodwas found to be rectilinear over the concentration range of 0.5-20.0 μg/mL for CIP, NOR or PHZ. These optimized and validated methods were successfully applied for the simultaneous analysis of the studied drugs in their synthetic mixtures and co-formulated tablets. Moreover, the second method was further extended to the determination of these drugs in human urine with direct injection and without any pretreatment. [ABSTRACT FROM AUTHOR]

In this study, a series of new, highly sensitive BF2-chelated tetraarylazadipyrromethane dyes are synthesized and analyzed to be suitable as on/off photo-induced electron transfer modulated fluorescent sensors for determination of intracellular pH. The ethanolic solutions of the new indicators feature absorption maxima in the range of 696–700 nm and a fluorescence emission maximum at 720 nm. Molar absorptivity and fluorescence quantum yield data were determined for the studied set of aza-BODIPY indicators. These indicators have high molar absorption coefficients of ∼80 000 M−1 cm−1 and quantum yields (up to 18%). Corresponding pKa values of indicators are determined from absorbance and fluorescence measurements and range from 9.1 to 10.8, depending on the selective positioning of electron-donating functionalities. The excellent photostability of the aza-BODIPY indicators makes them particularly suitable for long duration measurements. The in vitro cellular staining of living tissues in PC3 cells based on the isosbestic point at pH 7.8 and pH 9.3 has been employed which shows an increase in fluorescence intensity at 800 nm with increase in pH for certain compounds and fluorescence intensity decreases at 700 nm. Therefore, the new indicators are suitable for exploitation and adaptation in a diverse range of analytical applications. [ABSTRACT FROM AUTHOR]

A novel, specific, reliable, and accurate capillary zone electrophoretic method was developed and validated for the simultaneous determination of aliskiren hemifumarate, amlodipine besylate, and hydrochlorothiazide in their triple mixture dosage form. Separation was carried out in a fused-silica capillary (57.0 cm total length and 50.0 cm effective length, 75.6 μm internal diameter) by applying a potential of 17 kV and a running buffer consisting of 40 mM phosphate buffer at pH 6.0 with UV detection at 245 nm. The method was suitably validated with respect to specificity, linearity, LOD, and LOQ, accuracy, precision, and robustness. The method showed good linearity in the ranges 1-10, 2.5-25, and 30-300 μg/mL with LODs of 0.11, 0.33, and 5.83 μg/mL for amlodipine besylate, hydrochlorothiazide, and aliskiren hemifumarate, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their coformulated tablets. The results of the proposed method were statistically compared with those obtained by the RP-HPLC reference method revealing no significant differences in the performance of the methods regarding accuracy and precision. [ABSTRACT FROM AUTHOR]

One of the most common features of many different clinical conditions is pain; hence, there is a crucial need for eliminating or reducing it to a tolerable level to retrieve physical, psychological and social functioning. A first derivative synchronous spectrofluorimetry technique is proposed for the simultaneous determination of celecoxib and tramadol HCl, a recent coformulation authorized for treating acute pain in adults. The method includes using synchronous spectrofluorimetry at ∆λ = 80 nm where tramadol HCl was determined using first derivative technique at λ = 230.2 nm, while celecoxib was determined at λ = 288.24 nm. The proposed method was successfully applied to their co-formulated dosage forms in addition to spiked human plasma and validated in agreement with the guidelines of the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). The linear ranges were found to be 0.50-5.0 and 0.15-0.50, the limits of detection to be 0.088 and 0.011 and the limits of quantification to be 0.266 and 0.032 μg/ml for celecoxib and tramadol, respectively. Statistical analysis revealed no significant difference when compared with previously reported methods as evidenced by the values of the variance ratio F-test and Student t-test. The proposed method was successfully applied to commercial dosage forms and spiked human samples. Moreover, the greenness of the proposed method was investigated based on the analytical eco-scale approach, with the results showing an excellent green scale with a score of 95., (© 2024 John Wiley & Sons Ltd.)

Employing the Quality by Design paradigm through this work helped conclude the method operable design region for optimizing the high performance liquid chromatography (HPLC) assay using Design of Experiments and response surface methodology to obtain a good resolution and determination of all analysed compounds and to achieve a suitable analysis time. A deep understanding of the quality target product profile, analytical target profile and risk assessment for parameters that affect the method performance led to developing an accurate, precise and cost-effective method. Quality risk management principles were applied for determining the critical method parameters affecting the simultaneous determination of metformin hydrochloride (MET), linagliptin (LIN) and empagliflozin (EMP) by reversed-phase HPLC . The ternary mixture was successfully resolved in 5 min with a linearity range of (0.1-600) µg ml -1 for MET and (0.05-50) µg ml -1 for LIN and EMP. The newly developed method was validated according to the International Council for Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines. Good agreement was observed with the assay results of the reported UPLC one. To evaluate the greenness of the proposed method, an analytical Eco-Scale method was used., (© 2022 The Authors.)

Simple and rapid synchronous fluorometric methods were adopted and validated for the simultaneous analysis of a binary mixture of diphenhydramine (DIP) and ibuprofen (IBU) (Mix I) or DIP and phenylephrine (PHE) (Mix II) in their co-formulated pharmaceuticals without prior separation. Analysis of Mix I is based on the measurement of the peak amplitudes (D 1 ) of synchronous fluorescence intensities at 265.1 nm for DIP and 260 nm for IBU. The relationship between the concentration and the amplitude of the first-derivative synchronous fluorescence spectra showed good linearity over the concentration ranges 0.50-10.00 μg ml -1 and 0.50-7.90 μg ml -1 for DIP and IBU, respectively. Analysis of Mix II was based on measurement of the peak amplitude (D 1 ) synchronous fluorescence intensities at 230 nm for DIP and at 253.9 nm for PHE. Moreover, for Mix II, the peak amplitude (D 2 ) synchronous fluorescence intensities were measured at 227.9 nm for DIP and at 264.9 nm for PHE. Calibration plots were rectilinear over the concentration range 0.30-3.50 μg ml -1 and 0.03-0.75 μg ml -1 for DIP and PHE, respectively. The proposed methods were successfully applied to determine the studied compounds in pure form and in pharmaceutical preparations., (© 2020 John Wiley & Sons, Ltd.)