Simultaneous Determination Research Articles

Antioxidant and Pro-Oxidant Properties of Selected Clinically Applied Antibiotics: Therapeutic Insights.

The balance between antioxidants and pro-oxidants plays a significant role in the context of oxidative stress, influenced by both physiological and non-physiological factors. In this study, 18 prescribed antibiotics (including doxycycline hydrochloride, tigecycline, rifampicin, tebipenem, cefuroxime, cefixime, potassium clavulanate, colistin, ampicillin, amoxicillin, amikacin, nalidixic acid, azithromycin, pipemidic acid trihydrate, pivmecillinam, aztreonam, fosfomycin sodium, and ciprofloxacin) were subjected to simultaneous determination of antioxidant and pro-oxidant potential to assess if pro-oxidant activity is a dominant co-mechanism of antibacterial activity or if any antibiotic exhibits a balanced effect. This study presents a recently developed approach for the simultaneous assessment of antioxidant and pro-oxidant potential on a single microplate in situ, applied to prescribed antibiotics. Ten antibiotics from eighteen showed lower antioxidant or pro-oxidant potential, while five exhibited only mild potential with DPPH50 values over 0.5 mM. The pro-oxidant antioxidant balance index (PABI) was also calculated to determine whether antioxidant or pro-oxidant activity was dominant for each antibiotic. Surprisingly, three antibiotics-doxycycline hydrochloride, tigecycline, and rifampicin-showed significant measures of both antioxidant and pro-oxidant activities. Especially notable was tebipenem, a broad-spectrum, orally administered carbapenem, showed a positive PABI index ratio, indicating a dominant antioxidant over pro-oxidant effect. These findings could be significant for both therapy, where the antibacterial effect is enhanced by radical scavenging activity, and biotechnology, where substantial pro-oxidant activity might limit microbial viability in cultures and consequently affect yield.

A general and rapid LC-MS/MS method for simultaneous determination of voriconazole, posaconazole, fluconazole, itraconazole and hydroxyitraconazole in IFI patients

ObjectiveTo establish a rapid and universal quantitative liquid chromatography tandem mass spectrometry (LC-MS/MS) method for measuring the exposure levels of five triazole antifungal drugs in human plasma, including voriconazole, fluconazole, posaconazole, itraconazole, and hydroxyitraconazole. MethodsA triple quadrupole mass spectrometer operating in positive ionization mode was used to detect the analyte, and multiple reaction monitoring mode was employed to gather data. The mobile phase included 0.05 % formic acid in water (phase A) and acetonitrile (phase B). The analytes were separated on an Agilent EclipsePlusC18 RRHD column (30 × 50 mm, 1.8 μm) using gradient elution. The flow rate was 0.3 mL/min with the column temperature set at 35 °C. The acetonitrile was used to pretreat the plasma sample, and the itraconazole-D5 and hydroxyitraconazole-D5 were utilized as the internal standards. ResultsThe calibration range was from 100 to 10,000 ng/mL for posaconazole, itraconazole, and hydroxyitraconazole, from 200 to 20,000 ng/mL for fluconazole and from 50 to 5000 ng/mL for voriconazole, with linear correlation coefficients more than 0.99 for all regression curves. The intra- and inter-day accuracy and precision of the method were within ±15 %. The mean extraction recovery of all the analytes ranged from 74.32 % to 117.83 %, and the matrix effect was from 72.54 % to 111.2 %. The results of stability fell into the scope of ±15 % deviation. ConclusionThis newly developed method is sensitive, simple, and robust, and successfully applied in determining triazole antifungal drugs in plasma from 66 IFI patients to provide reference for safe and effective drug administration in clinical practice.

An environmentally sustainable synchronous spectrofluorimetric method coupled with second derivative signal processing for simultaneous determination of velpatasvir and simeprevir in pharmaceutical and plasma samples

Velpatasvir and simeprevir are two direct acting antivirals that are often used in combination with sofosbuvir to treat HCV infections. Herein, an environmentally benign spectrofluorimetric method was developed for simultaneous quantification of velpatasvir and simeprevir in pharmaceutical and plasma samples. To address the issue of overlapping fluorescence spectra presented by these compounds, this method integrates synchronous fluorescence and second-derivative spectroscopy. By employing the second derivative of the synchronous fluorescence spectra measured at Δλ of 140 nm, the accurate determination of velpatasvir at 400 nm and simeprevir at 426 nm was achieved without any interference. Different experimental parameters affecting the synchronous fluorescence of the studied drugs were carefully optimized. The plots of second-derivative amplitudes against concentrations showed linearity in the range of 5–400 ng/mL for velpatasvir and 80–800 ng/mL for simeprevir. The method was very sensitive, with lower detection limits of 1.11 ng/mL and 25.40 ng/mL, and quantification limits of 3.36 ng/mL and 76.96 ng/mL for velpatasvir and simeprevir, respectively.The method was effectively used to determine velpatasvir and simeprevir simultaneously in their pure forms, pharmaceutical dosage forms, and human plasma with no interference. The suggested technique was additionally evaluated for its eco-friendliness through the utilization of the Analytical GREEnness (AGREE) and Green Analytical Procedure Index (GAPI) evaluation metrics, revealing that the method is indeed sustainable.

High-sensitive electrochemical sensor based on Ni/NiCx-integrated functional carbon nanotubes for simultaneous determination of acetaminophen and dopamine

In complex environmental substance monitoring, the simultaneous detection of single and multiple substances with high sensitivity has been a research focus in the field of electrochemical sensors. Rational selection of appropriate dopants to optimize the electrode material is crucial in this regard. In this work, we employed a multi-doping strategy to effectively enhance the electrocatalytic performance of multi-walled carbon nanotubes (MWCNTs). By doping Ni/NiCx onto MWCNTs, we successfully constructed a heterojunction material (Ni/NiCx-N-MWCNTs). The successful doping of Ni/NiCx allows for the synergistic effects of multiple elements. Ni/NiCx serves as a conductive bridge, forming a three-dimensional network of nanotubes, which effectively reduces the aggregation of carbon nanotubes, exposes more active sites, and enhances electrocatalytic activity. The electrochemical sensor based on Ni/NiCx-N-MWCNTs demonstrated high sensitivity, selectivity, and simultaneous electrochemical detection for acetaminophen (1–150 μM, limit of detection (LOD)=0.56 μM) and dopamine (1–80.0 μM, LOD=0.19 μM). Its excellent reproducibility (relative standard deviation (RSD)=2.01 %) and interference resistance provide Ni/NiCx-N-MWCNTs with significant advantages over other electrode materials, indicating a promising application potential.

A Straightforward Electrochemical Approach for the Simultaneous Determination of Thymol and Carvacrol in Essential Oils

A novel, simple, rapid, and non-expensive analytical method based on square wave voltammogram at Pt-microelectrode coupled with partial least square multivariate calibration was used for the simultaneous quantitation of thymol (THY) and carvacrol (CAR) in thyme and oregano essential oils. Results demonstrated that the multivariate calibration method successfully exploited the first-order advantage, rendering highly satisfactory quantitative figures (average recoveries not statistically different than 100%). Moreover, the results agree well with those obtained from the official analytical method. Last, the method’s environmental sustainability was asserted using the AGREE metric, highlighting its eco-friendly nature. More importantly, the proposed analytical procedure does not require previous sample preparation or electrode surface modification. The results underscore the suitability of the method for determining THY and CAR in essential oils at low concentrations (LOD ~ 7.6 µM) with REP% below 5.6%, meeting the requirements of the green analytical chemistry.

A chemometric approach using I-optimal design for optimising Pb(II) removal using bentonite-chitosan composites and beads

This paper reports adsorption studies of Pb(II) ions onto Bentonite-Chitosan (Bt-Ch) composites or beads when using an I-optimal design experiment approach. Three adsorption factors (pH, adsorbent dosage, and initial concentration) were optimised whilst simultaneously investigating multiple adsorbents. The Bt-Ch composites and beads (type A and B) adsorbents were made using weight ratios 90%/10% and differed characteristically due to their preparation methods of solution blending and precipitation, respectively. A batch procedure was used for adsorption experiments, and the amounts of Pb(II) ions (adsorbed onto Bt-Ch composites/beads) were analysed using inductively coupled plasma optical emission spectrometry (ICP-OES). Adsorption experimental parameters were analysed and optimised by using a response surface method (I-optimal design) generated from Design-Expert® 13.0 software. The main achievements of this study were to intensify the understanding and application of I-optimal experimental designs, which allow simultaneous determination of adsorption capacities and efficiencies across multiple adsorbents in an economical manner. A reduced quadratic model provided the best fit for the experimental data and exhibited minimal deviation between predicted and experimental values. This was evidenced by the very small covariance (CV) values of 1.81% and 1.33% observed for adsorption capacity and adsorption efficiency, respectively, also suggesting high reproducibility. It was observed that the adsorption factors studied (pH, adsorbent dose, and initial concentration) have a more pronounced effect on the adsorption capacity (F-value = 714.37) compared to adsorption efficiency (F-value = 140.62). Adsorbent dosage was found to have the greatest effect on adsorption capacity, while the initial pH of Pb(II) solution had the greatest effect on adsorption efficiency. Under optimal conditions, the adsorption capacities of beads-A (73.2 mg/g) and beads-B (77.6 mg/g) were found to be higher than that of the corresponding composite (51.7 mg/g). Whilst the optimum adsorption efficiency values for all three adsorbents were ∼100% (with ranges of pH 2–5, initial concentrations 50–200 mg/L, and adsorbent dosage 0.05–0.5 mg). The desirability indexes for the optimised conditions for these respective responses (and each adsorbent) were found to be within the ranges of 0.892–0.974 and 0.945–0.967 for adsorption capacity and adsorption efficiency, respectively. These high desirability index values for both responses indicate that the optimised conditions lead to very good performance for both measures. The information obtained in this study provides detailed understanding of the adsorption phenomena of the adsorbents studied. It gives confidence in the use of I-optimal designs to be applied as a chemometric tool for the specific adsorbents studied herein and others.

Simultaneous smartphone-based colorimetric determination of melamine and sodium hypochlorite in milk samples using a simple microfluidic kit

Simultaneous smartphone-based colorimetric determination of melamine and sodium hypochlorite in milk samples using a simple microfluidic kit

Development and Validation of Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Citicoline and Nimodipine in Bulk and Tablets

Development and Validation of Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Citicoline and Nimodipine in Bulk and Tablets

A green and sensitive electromembrane extraction (EME) method for the determination of dialkylphosphates in maternal urine and amniotic fluid

Organophosphates compounds are extensively used pesticides, whose metabolites, dialkyl phosphates, are considered as bioindicators of human exposure. Recently, research has indicated that they can affect thyroid endocrine function. Pregnant women are a particularly vulnerable cohort to these effects due to concerns about prenatal exposure to environmental pollutants. For the first time an electromembrane microextraction method is proposed for the simultaneous determination of seven dialkylphosphate metabolites in maternal urine and amniotic fluid, which is compatible with mass spectrometry detection and achieves highly sensitive levels of quantitation. Dialkylphosphates were extracted from a 10 mL donor solution at pH 7 into a 50 µL acceptor solution at pH 12 using 1-octanol as the supported liquid membrane and applying 60 V for 10 min at 600 rpm. The obtained extracts were analysed by ion pair liquid chromatography coupled to a triple quadrupole mass spectrometer, using an Acquity UPLC® BEH C18 column (100 mm × 2.1 mm i.d., 1.7 µm particle size) at 30 °C. Under optimal extraction conditions, the preconcentration factors were achieved were up to 178-fold, allowing for high sensitivity levels, in the order of ng mL−1. The limits of quantitation were within 0.075 ng mL−1 (diethyl thiophosphate) and 1.67 ng mL−1 (dimethyl phosphate) in maternal urine samples and within 0.015 ng mL−1 (diethyl thiophosphate) and 0.5 ng mL−1 (dimethyl dithiophosphate) in amniotic fluid samples. The comparative study revealed a significant improvement in terms of analysis time, sensitivity, greenness, and practicality. Finally, the applicability of the method for the determination of selected dialkylphosphates was demonstrated in paired maternal urine and amniotic fluid samples. These results suggest potential placental transfer to the offspring.

Determination of 22 elements in whole blood by inductively coupled plasma mass spectrometry

Objective: To establish a method for the simultaneous determination of 22 elements, including beryllium, vanadium, chromium, manganese, iron, calcium, magnesium, barium, cobalt, cadmium, copper, zinc, arsenic, selenium, titanium, strontium, nickel, molybdenum, tin, antimony, thallium and lead, in whole blood by inductively coupled plasma mass spectrometry (ICP-MS) . Methods: In September 2023, the analysis conditions were determined by optimizing the detection mode of the instrument, the pretreatment mode and the dilution factor of the samples, etc. Whole blood samples were diluted with a mixture of 0.1% nitric acid and 0.05% triton X-100, and centrifuged at 2000 r/min by high-speed centrifuge for 2 min. The supernatant was taken into inductively coupled plasma mass spectrometer to determine the content of 22 elements, and the detection limit and precision of the method were analyzed. Results: The 22 elements had a good linear relationship in their respective measurement ranges (r=0.9991-0.9999), the detection limit ranged from 0.003 μg/L to 0.012 mg/L. The intra-batch precision ranged from 0.5% to 7.2%, the inter-batch precision ranged from 0.4% to 9.4%, and the average recoveries ranged from 80.6% to 114.9%. Conclusion: ICP-MS method has a good effect on the determination of 22 elements in whole blood. The method is fast and simple, and can be used for clinical detection of multiple elements in whole blood.

Development and Validation of Novel RP-HPLC Method for the Simultaneous Estimation of Itraconazole and Secnidazole in Bulk and Pharmaceutical Formulations

Simple, accurate and precise RP-HPLC method for the simultaneous estimation of Itraconazole (ITZ) and Secnidazole (SEC) in bulk and pharmaceutical formulations has been developed and validated. The chromatographic analysis was performed on Shimadzu model equipped with SPD-20 AD UV detector, isocratic pump LC- 20 AD and loop injector. The chromatographic separation was performed using C18 column (250mm x 4.6mm i.d. and 5µm particle size). The analytes were monitored at 257nm using methanol: potassium dihydrogen phosphate buffer (PDP) pH 5.5 in the ratio of 90:10v/v with a flow rate of 1.5ml/min. The retention time was found to be 6.037 min for ITZ and 3.788 min for SEC. The linearity was found to be in the range of 10-50µg/ml for both ITZ and SEC with a regression coefficient of 0.999 and 0.998 for ITZ and SEC respectively. The method was validated in accordance with ICH guidelines for its linearity, precision, accuracy, robustness, ruggedness, LOD and LOQ. The recovery studies were carried out which confirmed the accuracy of the proposed method. LOD values for ITZ & SEC was found to be 0.583µg/ml and 0.241µg/ml, respectively. LOQ values for ITZ and SEC was found to be 1.749µg/ml and 0.732µg/ml, respectively. The developed method was also found to be precise and robust for the simultaneous determination of ITZ and SEC in bulk and pharmaceutical formulations.

Trifluoroacetic acid modified MOF-808 composite coating for solid-phase microextraction of six phenols followed by gas chromatography analysis

The development of adsorption materials with good stability and high efficiency is significant in solid-phase microextraction (SPME). In this work, metal–organic framework MOF-808 (Zr) was modified by trifluoroacetic acid (TFA) to improve its hydrophobicity. MOF-808-TFA was electrochemically deposited on stainless steel wire with poly (3, 4-ethylenedioxthiophene) (PEDOT) to increase its extraction efficiency. The main parameters in the synthesis and extraction procedure were optimized. The prepared MOF-808-TFA@PEDOT nanocomposite coating was characterized by scanning electron microscopy, energy dispersive spectrometer, X-ray diffraction, Fourier transform infrared spectrometry and thermogravimetric analysis. A direct immersion solid-phase microextraction (DI-SPME) method for six phenols was developed based on the nanocomposite coating which had good service life (150 times). The extraction efficiency was 12 times higher than the commercial PDMS coating. Combined with gas chromatography-flame ionization detector (GC-FID), a simultaneous determination method for the six phenols was established, which exhibited wide linear range with 0.05–50 μg L−1 (R2 > 0.99). The limit of detection was 0.01–0.08 μg L−1 (S/N = 3), and the limit of quantification was 0.05–0.25 μg L−1. The method was applied to determine the migration quantity of phenols from four metal cans with recovery rate between 85.6–116.8 % (RSD < 13.9 %), and it was verified by standard GC–MS method and SPSS statistical analysis. These results indicated the DI-SPME-GC-FID method had reliability and potential application in security testing for food contact materials.

Simultaneous Determination of Ethanol and Methanol in Wines Using FTIR and PLS Regression.

Accurate quantification of ethanol and methanol is essential for regulatory compliance and product quality assurance. Fourier Transform Infrared Spectroscopy (FTIR) offers rapid, non-destructive analysis with minimal sample preparation, making it a promising tool for wine analysis. In this exploratory study, the use of FTIR and PLS regression for the simultaneous quantification of ethanol and methanol in wine samples of 11 different Portuguese mono-varietal wines and different vintages deriving from the same winery in Lisbon was investigated. A model was developed, demonstrating the feasibility of FTIR and PLS regression for the simultaneous quantification of ethanol and methanol in wine samples through dedicated models; it showed good prediction capacity for ethanol determination but poorer performance for methanol quantification. The model could be reliable enough for quality control in wine production, but to improve its performance should be enhanced in the future with more samples from different origins, wine types, and a wider concentration range in the case of methanol.

“Eco-friendly HPLC method for analysis of dipyrone and hyoscine in different matrices with biomonitoring”

A selective, precise, and accurate reversed HPLC method has been developed and validated for simultaneous separation and determination of two veterinary drugs, dipyrone and hyoscine, in their combined dosage form in the presence of their official impurities, namely 4-aminoantipyrine and tropic acid, in addition to the formulated preservative: phenol. The linearity range was found to be (1.00–35.00 µg/mL) for dipyrone and (2.50–50.00 µg/mL) for hyoscine. It exhibited a satisfactory linearity regression R (0.9999) for both drugs with LOD 0.22 µg/mL and 0.72 µg/mL and LOQ 0.65 µg/mL and 2.19 µg/mL for dipyrone and hyoscine, respectively. Additionally, the two cited drugs were also determined in the presence of dipyrone active metabolite 4-aminoantipyrine using diclofenac as an internal standard in bovine urine. The linearity range was found to be (15–75 µg/mL) for dipyrone, (2.5–60 µg/mL) for hyoscine, and (2.5–60 µg/mL) for 4-aminoantipyrine with linearity regression R (0.9999–0.9998). The LLOQ (15, 2.5, 2.5 µg/mL), LQC (45, 7.5, 7.5 µg/mL), MQC (55, 25, 25 µg/mL), and HQC (60, 50 50 µg/mL) were determined for dipyrone, hyoscine and 4-aminoantipyrine, respectively. UV detection was carried out at 220 nm. The method was validated according to the ICH guidelines, as well as according to FDA guidelines for determining both drugs in bioanalytical matrices and both proved accuracy and precision. A statistical comparison was made between the results obtained and those obtained by the reported method, showing no significant difference in accuracy and precision at p = 0.05. The suggested method was proved eco-friendly through a greenness assessment using two different tools (The analytical eco-scale scored 83, and the AGREE-Analytical Greenness Metric approach scored 0.83). The suggested method can be used in the routine work of quality control labs, screening for drug abuse, and ensuring clean sport for horse racing.

Development of a Simultaneous HPLC Determination Method of Cacao Polyphenols, Caffeine and Theobromine in High Cacao Chocolate by Core-Shell Type Reversed-Phase Columns

Development of a Simultaneous HPLC Determination Method of Cacao Polyphenols, Caffeine and Theobromine in High Cacao Chocolate by Core-Shell Type Reversed-Phase Columns

UPLC-PDA factorial design assisted method for simultaneous determination of oseltamivir, dexamethasone, and remdesivir in human plasma

A green and simple UPLC method was developed and optimized, adopting a factorial design for simultaneous determination of oseltamivir phosphate and remdesivir with dexamethasone as a co-administered drug in human plasma and using daclatasvir dihydrochloride as an internal standard within 5 min. The separation was established on UPLC column BEH C18 1.7 μm (2.1 ×\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\ imes $$\\end{document} 100.0 mm) connected to UPLC pre-column BEH 1.7 μm (2.1 ×\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\ imes $$\\end{document} 5.0 mm) at 50 °C with an injection volume of 10 μL. The photodiode array detector (PDA) was set at three wavelengths of 220, 315, and 245 nm for oseltamivir phosphate, the internal standard, and both dexamethasone and remdesivir, respectively. The mobile phase consisted of methanol and ammonium acetate solution (40 mM) adjusted to pH 4 in a ratio of 61.5:38.5 (v/v) with a flow rate of 0.25 mL min−1. The calibration curves were linear over 500.0–5000.0 ng mL−1 for oseltamivir phosphate, over 10.0–500.0 ng mL−1 and 500.0–5000.0 ng mL−1 for dexamethasone, and over 20.0–500 ng mL−1 and 500.0–5000.0 ng mL−1 for remdesivir. The Gibbs free energy and Van't Hoff plots were used to investigate the effect of column oven temperatures on retention times. Fluoride-EDTA anticoagulant showed inhibition activity on the esterase enzyme in plasma. The proposed method was validated according to the M10 ICH, FDA, and EMA’s bioanalytical guidelines. According to Eco-score, GAPI, and AGREE criteria, the proposed method was considered acceptable green.

Development and validation of a green spectrophotometric method for simultaneous determination of combined pharmaceutical dosage form (paracetamol and caffeine) using chemometrics technique in comparison with HPLC

Development and validation of a green spectrophotometric method for simultaneous determination of combined pharmaceutical dosage form (paracetamol and caffeine) using chemometrics technique in comparison with HPLC

Electrochemical immunoplatform for the determination of multiple salivary biomarkers of oral diseases related to microbiome dysbiosis

Several diseases of the oral cavity are related to compositional and functional shifts in the oral microbiome. The analysis of saliva is an attractive alternative for the diagnosis and prognosis of these diseases. Samples can be obtained by no invasive procedures and processing is relatively simple. However, sensitive and selective analytical methods are needed to make the diagnosis as specific as possible. In this work, four salivary biomarkers of oral diseases: interleukin-6 (IL-6), receptor activator of NF-kB ligand (RANKL), protein arginine deiminase 4 (PAD4) and the corresponding antibody (anti-PAD-4) were selected as targets for their simultaneous determination using an electrochemical immunosensing platform. Sandwich-type amperometric immunoassays were implemented using horseradish peroxidase (HRP)/H2O2/hydroquinone (HQ) for application to the analysis of saliva of six volunteers. The developed method provides excellent sensitivity, selectivity, and wide linear ranges with LOD values of 0.09 pg mL−1 (IL-6), 0.10 pg mL−1 (RANKL); 0.09 ng mL−1(PAD4) and 14.5 ng mL−1 (anti-PAD4) and allows the accurate analysis of saliva without matrix effects, using 25 μL of raw sample. The developed methodology is competitive with commercial ELISA kits available only for a single biomarker determination, while the assay for the four biomarkers can be completed in less than two hours.

MOF derived ZnCo2O4@nitrogen-doped carbon as an electrochemical sensor for simultaneous detection of acetaminophen and p-aminophenol

In this study, a rapid and sensitive electrochemical sensor (ZnCo2O4@NC) based on metal-organic frame (MOF)-derived metal oxide material (ZnCo2O4) and chitosan derived nitrogen-doped carbon material (NC) was successfully constructed for the simultaneous determination of acetaminophen (APAP) and p-aminophenol (PAP). A series of electrochemical experiments proved that the MOF derived ZnCo2O4@NC composite has excellent electrochemical response to APAP and PAP in the phosphate buffer saline (PBS) (pH 7.0). The current response varies linearly with the increase of APAP concentration in the range of 8.0 μmol L−1 to 520 μmol L−1 and PAP concentration in the range of 6.0 μmol L−1 to 420 μmol L−1. The sensitivity and limit of detection (LOD) of ZnCo2O4@NC for APAP and PAP detection are 0.1024 and 0.2749 μA μmol L−1 cm−2, 0.0608 and 0.2489 μmol L−1, respectively. The ZnCo2O4@NC composite modified electrode exhibits good selectivity, reproducibility and stability. Additionally, in the detection for acetaminophen sustained-release tablets, the recovery rates of APAP are in the range of 90.00 % –100.00 %. The theoretical content is consistent with our detection results, showing that this method has good accuracy in actual sample analysis. This study provides an innovative idea to improve electrochemical performance of simultaneous detection of acetaminophen and p-aminophenol through the comprehensive strategy of structural design, heteroatom doping.

Rapid UV-Vis spectrophotometric method aided by firefly-PLS models for the simultaneous quantification of ciprofloxacin, lomefloxacin, and enrofloxacin in their laboratory mixture, dosage forms and water samples: greenness and blueness assessment

Herein, a novel UV spectrophotometric method coupled with chemometric tools was developed for the simultaneous determination of three fluoroquinolone antibiotics: ciprofloxacin, lomefloxacin, and enrofloxacin. Such integration of UV spectroscopy and chemometric analysis proved to be a simple, rapid, and cost-effective approach for the quantification of these clinically important pharmaceutical compounds and aid in their quality control analysis. The method employed firefly algorithm for variable selection and partial least squares (PLS) regression for model calibration. The developed method was validated by independent test set in addition the accuracy, intra and inter-day precision as per ICH guidelines which showed a satisfactory performance with mean recovery ranged between 98.18 and 101.83 with %RSD < 2. Besides, the developed method displayed ultrasensitive levels with LODs (0.0803, 0.1125, 0.1309 µg/mL) and LOQs (0.2434, 0.3409, 0.3968 µg/mL) for ciprofloxacin, lomefloxacin, and enrofloxacin, respectively. The greenness and blueness of the developed method were also evaluated using the recently proposed Analytical GREEnness metric approach (AGREE) and Blue applicability grade index (BAGI) tools, which showed a high AGREE score of 0.79 and a BAGI score of 77.5. These results indicate that the developed method provides an environmentally friendly alternative to the traditionally used chromatographic techniques, while maintaining high analytical practicability. Finally, the application of the developed methodology was demonstrated on real pharmaceutical and tap water samples, and the results were in good agreement with those obtained by the reference HPLC method indicating the reliability and suitability of the proposed spectrophotometric method for routine analysis of fluoroquinolone antibiotics.