Background This in vitro study evaluated monomer release from different light-cured composites used for clear aligner attachments over time, assessing the effects of composite type, attachment size and curing duration. Methods Four composite materials (3M™ Filtek™ Supreme Flowable, 3M™ Filtek™ Z350 XT Universal, 3M™ Transbond™ XT, and Tokuyama Estelite Posterior) were shaped into attachment-like specimens using 3D-printed molds with heights of 3 mm, 4 mm, and 5 mm. Polymerization was performed using a VALO LED curing unit with two curing protocols (6 s and 12 s). Monomer release was quantified at 1 hour, 1 day, 7 days, and 14 days using high-performance liquid chromatography (HPLC). Statistical analyses were performed using Kruskal–Wallis and post-hoc Bonferroni tests (p < 0.05). Results Intragroup analyses demonstrated significant height- and time-dependent differences in TEGDMA and Bis-GMA release for all composites under both curing protocols (p < 0.001). Under 6 s curing, monomer release increased with specimen height, whereas 12 s curing reduced early elution and yielded more stable profiles. Intergroup comparisons revealed significant differences among composites at all heights, curing durations, and time points (mostly p < 0.001). Conclusion Light-curing duration, attachment size, and composite type significantly influence monomer release.

This study introduces a combined HPLC and UV detection technique for the quantification of casticin in capsule and human plasma samples. The chromatographic separation was carried out utilizing a C18 column (150 mm & times; 4.6 mm & times; 5 mu m) at a temperature of 25 degrees C. Isocratic elution with a mobile phase comprising 60:40 v/v (methanol-0.05% formic acid) was employed. Flow rate was adjusted 1 mL/min. The analyte was determined at a wavelength of 258 nm, with a retention time of 14.7 +/- 0.01 min. The developed method underwent validation according to ICH criteria, covering specificity, linearity, precision, accuracy, detection and quantitation limits, as well as robustness. The linear range was determined to be 10-60 ng/mL for both capsule and spiked plasma specimens. The suggested technique was performed to the analysis of casticin in spiked human plasma and pharmaceutical preparations, yielding a recovery of 106.04% and demonstrating precision through intra-day and inter-day experiments with the highest relative standard deviation (RSD %) value of 4.94. Consequently, the technique was performed to the quantifying of human plasma specimens from in a patient taking medication containing casticin.

Two novel high-performance liquid chromatography (HPLC) methods were developed and validated for the determination of dolutegravir (DTG), lamivudine (3TC), and abacavir (ABA) in pharmaceutical formulations. In this study, AI engines such as Copilot, ChatGPT 5.2, Gemini, and Perplexity were integrated into HPLC method development. The selected predicted conditions underwent experimental optimization, validation, and refinement. Their practical implementation significantly improved efficiency and accuracy in the analytical process. The first method, an isocratic HPLC, was designed for the simultaneous quantification of DTG and 3TC using an XBridge® C18 column and a mobile phase of acetonitrile:phosphate buffer (pH 3.5, 50:50 v/v). Detection was performed at 258.0 nm for DTG and 275.0 nm for 3TC. The second method, a gradient HPLC, enabled the simultaneous quantification of DTG, 3TC, and ABA on a Spherisorb® ODS2 C18 column with methanol and TEA/TFA buffer (pH 3.15) as the mobile phase. Detection wavelengths were 258.0, 278.0, and 294.0 nm for DTG, 3TC, and ABA, respectively. The calibration ranges were wide and showed excellent linearity. Both techniques were validated in accordance with ICH Q2(R2) guidelines. The approaches align with smart analytical chemistry principles, combining green and white analytical chemistry (GAC and WAC) with AI-driven method development, resulting in accurate, fast, and sustainable techniques suitable for routine quality control applications.

Artificial Intelligence (AI) is revolutionizing analytical chemistry by promising rapid method development, yet its real-world efficacy remains untested in complex pharmaceutical separations. This study leverages AI to design an HPLC method for Amlodipine (AMD), Hydrochlorothiazide (HYD), and Candesartan (CND), comparing it with an experimentally optimized approach to uncover practical benefits and limitations. Our findings reveal AI's potential to accelerate innovation while highlighting the critical role of human expertise. The In-Lab optimized HPLC method utilized an Xselect CSH Phenyl Hexyl (R) (2.5 mu m, 4.6 x 150 mm) column with a mobile phase of acetonitrile:water (0.1 % trifluoroacetic acid) (70:30, v/v), a flow rate of 1.3 mL/min, and UV detection at 250 nm. It achieved rapid elution with retention times of AMD = 0.95 min, HYD = 1.36 min, and CND = 2.82 min. The AI-generated method used a C18 column (5 mu m, 150 mm x 4.6 mm), gradient elution with phosphate buffer (pH 3.0) and acetonitrile, a flow rate of 1.0 mL/min, and detection at 240 nm, resulting in longer retention times: AMD = 7.12 min, HYD = 3.98 min, and CND = 12.12 min. Linearity ranges were AMD (25.0-250.0 mu g/mL), HYD (31.2-287.0 mu g/mL), and CND (40.0-340.0 mu g/mL) for the In-Lab method, and AMD (30.0-250.0 mu g/mL), HYD (35.0-285.0 mu g/mL), and CND (50.0-340.0 mu g/mL) for the AI-HPLC method. Both approaches were validated per ICH guidelines, confirming specificity, accuracy, and reliability. The obtained results were statistically compared with the reported ones using the F-test and Student's t-test. In terms of sustainability, the In-Lab method outperformed the AI-based method according to MoGAPI, AGREE, and BAGI assessments, due to reduced solvent use, waste generation, and analysis time. This study underscores the necessity of human intervention to refine AIgenerated methods, aligning them with both analytical efficiency and green chemistry goals. Improving AI tools to predict optimal HPLC conditions is essential for advancing sustainable and effective analytical practices.

Green Analytical Chemistry (GAC) aims to create eco-friendly methods for pharmaceutical analysis, with a focus on quality control. This study focuses on the simultaneous quantification of candesartan (CAN), hydrochlorothiazide (HCT), and amlodipine (AML) in a triple medication using two green spectrophotometric techniques. The study incorporates mathematical manipulation approaches to extract the parent spectrum of each drug component. These integrated methods address the problem of spectral signal overlap without requiring prior separation, utilizing a factorized spectrum (FS), which is notable for its capacity to assess the specified drugs in the mixture and retrieve their original zero-order spectra it is distinctive for its ability to evaluate the mentioned drugs within the mixture and recover their initial zero-order spectra. The first integrated resolution technique, the Integrated signal processing plan (ISPP-D0), was applied to the mixture's zero-order spectrum, including successive manipulation of three methods: extended absorbance difference, absorbance resolution, and spectrum subtraction. The second integrated resolution technique is the Integrated signal processing plan (ISPP-R)via ratio spectrum of the mixture, which includes successive manipulation of three methods: dual amplitude difference, ratio extraction, and spectrum subtraction. The proposed methods were validated and assessed following the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) guidelines, showing linear concentration ranges of 5.0-35.0 µg/mL for CAN at 254.0 nm, 2.0-20.0 µg/mL for HCT at 270.0 nm, and 5.0-35.0 µg/mL for AML at 240.0 nm. The specificity was evaluated by accurately and precisely determining the concentrations of the three drugs in their synthetic blends and single-tablet pharmaceutical formulation. The findings were statistically analyzed against the official results using the F-test and Student's t-test, indicating no notable differences. These UV spectrophotometric techniques align with green analytical chemistry (GAC) and white analytical chemistry (WAC) principles, supporting the United Nations Sustainable Development Goals (UNSDGs). These integrated analytical techniques for drug analysis offer enhanced precision and efficiency, enabling the retrieval of zero-order spectra that serve as unique fingerprints for each analyte. These advancements simplify the identification process, improve accuracy, and ensure reliable results, making them invaluable in pharmaceutical research and quality control.

This study presents a combination of High Performance Liquid Chromatography (HPLC) and ultraviolet (UV) detection that provides the quantification of agnuside in human plasma specimens. Reverse-phase chromatographic separation was carried out with C18 column (150 mm x 4.6 mm x 5 mu m), at 25 degrees C with isocratic elution of the mobile phase containing methanol: 0.1% formic acid (35:65 v/v) at 0.6 mL/min flow rate. Experiments were carried out at a wavelength of 258 nm. The retention time of the analyte is 9.70 +/- 0.01 min. The developed technique was validated based on the International Conference on Harmonization guideline. The correlation coefficient of the technique was 0.9915, and the calibration range was 5-125 mu g/mL. The recovery value of the proposed method was found to be 101.4%, and the precision of the method was calculated as 6.35 with the highest RSD% value. A pharmacokinetic study was performed by administering agnuside to a healthy volunteer.

The greening of analytical methods has gained interest in the field of quantitative analysis to reduce environmental impact and improve analyst's safety and health. For postmenopausal women with hormone-responsive advanced breast cancer, Letrozole (LTZ) has been a standard first-line endocrine therapy A green HPLC method was developed, optimized, validated, and applied for quantification of the LTZ in tablets. Experiments were conducted on the Inertsil ODS- 3 (R) C18 (5 mu m, 150 x 4.6 mm). An isocratic elution was applied using a mobile phase consisting of ethanol: water (50:50, v/v). A wavelength of 230.0 nm was chosen for the analysis. An experiment was finished 3.0 mins. Calibration graphs for each drug were rectilinear in the range of 0.1 - 40.0 mu g/ mL. Validation studies were carried out based on International Conference on Harmonization (ICH) recommendations. The student (t) test for means and the (F) test for standard deviations were used to compare the results. In this study, we utilized the ChlorTox Scale, Greenness Index, AGREE, GAPI, and NQS Indicator to comprehensively evaluate the environmental, safety, and sustainability aspects of analytical methodology, aligning our approach with the United Nations Sustainable Development Goals (SDGs). It can be applied to quality control, bioequivalence studies, and routine analysis.

A novel simple and cost effective HPLC technique was presented for the quantification of selexipag (SLP) in human plasma sample and the technique's applicability to a pharmacokinetic investigation. Chromatographic separation was achieved with C1 8 (5 mu m 3 4.6 mm 3 150 mm) column, at 30 8C with isocratic elution, mobile phase composed of solution A (acetonitrile), and solution B (0.5% formic acid) (65:35 v/v) at flow rate 1.2 mL min-1. The linearity range is 10-150 ng mL-1. As sample preparation step human plasma was precipitated with acetonitrile and the detection was provided at 300 nm. The retention time is 8.20 +/- 0.02 min. LOD is found to be 3.3 ng mL-1 for drug. The method was applied to the analysis of SLP in human plasma with good recovery as 97.83%. Validation of the studied methods was carried out according to EMA guideline. The new method applied on a prototype pharmacokinetic study by administration of 800 mu g SLP to a healthy volunteer and parameters like AUC0-24, AUC0-infinity, Cmax, tmax, and t1/ 2 were assessed.

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A novel high performance liquid chromatography (HPLC) and spectrophotometric analysis were applied for quantification of active substances of sacubitril (SAC) and valsartan (VAL). HPLC experiments were conducted on the Waters Spherisorb (R) (3.0 mu m 60.0x4.0 mm) column. Preparation of mobile phase A: 200 mL of 0.1 % solution of trifluoroacetic acid in water and 800 mL of 0.1 % solution of trifluoroacetic acid in acetonitrile by volume are mixed. Preparation of mobile phase B: 800 mL of a 0.1 % solution of trifluoroacetic acid in water and 200 mL of 0.1 % solution of trifluoroacetic acid in acetonitrile by volume were mixed. It was given to the system at the ratio of Mobile Phase A: Mobile Phase B (35:65 v:v). The specimen was injected into the column at 15.0 mu L. A detection wavelength of 254.0 nm was preferred for the compound and the flow rate was 2.0 mL/min. Analysis was completed in 4.0 min. The column oven temperature was adjusted to 40.0( degrees)C. The methods were evaluated in terms of green chemistry. The methods have been validated according to ICH guidelines. For HPLC method calibration graphs were constructed in the 20.0- 145.0 and 20.0 - 155 mu g/mL SAC and VAL respectively with an R2 of 1.000. In recovery experiments, the RSD values were calculated to be 0.08 % and 0.34 % for SAC and VAL, respectively. Additionally, in intraday and interday experiments, percent RSD values were found to be between 0.23 and 0.49. The method developed for the analysis of the active substances has been developed with a short analysis time and is cost effective. SAC and VAL were determined using a novel method for spectrophotometric analysis. The determination was performed simultaneously using the applied method. This method is a constant center method. Calibration graphs were constructed in the 2.0- 20.0 and 2.0 - 25 mu g/mL SAC and VAL with an R2 of 0.9998 and 0.9999 respectively. It is a greenness method in terms of the analysis time and solvent used.

A novel analytical method based on ultra-fast liquid chromatography using fluorimetric detector was developed and validated for determination of non-steroidal anti-inflammatory drugs (NSAIDs) (ibuprofen (IBP), etodolac (ETD), dexketoprofen (DKP), sodium diclofenac (SDCF), and naproxen (NPX) in tap water, urine and pharmaceutical samples. Precolumn derivatisation of targeted NSAIDs was carried out with 4-bromomethyl-7-methoxy coumarin (BrMmC) using dibenzo-18-crown-6-ether as reaction catalyst leading to the formation of a fluorescent compound. The obtained fluorescent compound of NSAIDs were measured at excitation wavelength as 325 nm, and emission wavelength of 395 nm. Optimum analytical conditions were carefully studied and improved. C18 column, with the dimensions of 4.0 x 100 mm and 3 mu m particle size, was used. Gradient elution with methanol: water 40:60; v/v (eluent A) and acetonitrile 100% (eluent B) were used as mobile phase and flow rate of 0.4 mL/min. The linearity range of the analytes were between 0.01-10.0 mu g mL(-1). Recovery values obtained from pharmaceutical preparations were found as 100.04%, 99.99%, 100.09%, 99.98% and 100.47% for IBP, ETO, DKP, SDCF, NPX, respectively. LOD values were found to vary between 0.00009 mu g mL(-1) and 0.00048 mu g mL(-1) in tap water, urine and pharmaceutical samples. The optimised technique was successfully applied for the determination of NSAIDs in tap water, urine, and pharmaceutical specimen. The specified NSAIDs were not found in real tap water samples.

A new high-performance liquid chromatography (HPLC) method was applied for the quantification of the active substance of tofacitinib. Analysis was performed on a Chromasil 100 C18 (100.0 × 4.0 mm, 3.5 μm) stationary phase. The mobile phase consisted of acetonitrile:0.2% phosphoric acid in water (12:88, v/v). The prepared sample (20.0 μL) was injected into the system. A detection wavelength of 285.0 nm was chosen for the compound, and the flow rate was 0.8 mL/min. The experiment was completed in 5.0 min. The analysis temperature was set to 40.0°C. The method was evaluated using green chemistry. The method was validated according to the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines. For linearity studies calibration curves were constructed in the range of 10.0-200.0 μg/mL. The recovery values were calculated at 97.66% and 105.68%. The method developed for the analysis of the active substance had a short analysis time and was cost-effective. It is an environmentally friendly method due to the mobile phase content used. The technique can be used in laboratory analysis and bioequivalence experiments.

Objective: In our study, the simultaneous determination of fluoxetine (FLX) and olanzapine (OLZ) was performed by absorbance subtraction and absorbance correction spectrophotometric methods. Material and Method: The active substances were determined by choosing the isosbestic point of 232 nm in the absorbance subtraction method and 255 nm and 245 nm wavelengths in the absorbance correction method. The accuracy of the methods was determined by applying the percentage recovery studies to the laboratory mixtures. The percent recovery values were found in the range of 98.1-100.2 for OLZ and 96.8-105.3 for FLX. The concentration range studied was 3.12-15.62 and 3.45-17.28 µg/ml for OLZ and FLX, respectively. Result and Discussion: In the study, two active substances used in antidepressant treatment were determined simultaneously. Today, these active substances used in the treatment have started to be used in combination in order to achieve a better effect of the treatment. Therefore, simultaneous analysis of two active substances becomes important. Two different spectrophotometric methods were used for analysis. The methods have been successfully applied and validated for the simultaneous determination of antidepressant active substances. Since the applied methods do not require pre-separation and can be applied directly, the amount of waste generated is reduced. Environmentally sensitive methods have been applied.

Introduction: In this study, a new high performance liquid chromatographic method was developed to determine the amount of allicin (AL) and s-allyl cysteine (SAC) in Allium sativum L. extracts. Methods: In the method, C18 column (5 mu m x4.6 mm x150 mm) was used as the stationary phase at 25 degrees C and acetonitrile: water (70:30, v/v) mixture was used as mobile phase with 1 mL/min flow rate. Isocratic elution was applied. The injection volume was 20 mu L. Measurements were carried out at 254 nm with ultraviolet detection. Retention times for AL and SAC were 1.1 and 2.4 min, respectively. The method was validated according to International Conference on Harmonization criteria. Results: The limit of detection values for AL and SAC were 0.6 mu g/ mL and 1.5 mu g/mL, respectively. The limit of quantitation values for AL and SAC were 2 mu g/mL and 5 mu g/mL, respectively. The linearity of the method was between 2-100 mu g/mL and 5-30 mu g/mL for AL and s-allyl cysteine, respectively. The developed method was also validated and applied to three different trade extracts. Conclusion: This new method, which is quite fast, simple and economical, can be used in the analysis of Allium sativum L. extracts, which are named as black garlic in the contents of food supplements.

This research describes a simple, sensitive, and disposable modified glassy carbon electrode constructed using platinum nanoparticles anchored on reduced graphene oxide nanocomposite as a conductive modifier (Pt@rGO/ GCE) to detect an anti-coronavirus drug, Favipiravir (FAV). The as-synthesized nanocomposite was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), and atomic force microscopy (AFM). Under optimized conditions, the square wave voltammetry (SWV) method was used to determine trace amounts of FAV in real samples. The proposed electrode demonstrated a wide linear concentration range of 3.16 to 100.0 mu M with a low detection limit (LOD) of 2.46 mu M. Moreover, the developed electrode showed outstanding selectivity in the presence of several interferences with high repeatability and reproducibility. Finally, the developed electrode was applied to detect FAV in human plasma and pharmaceutical samples.

An HPLC method with UV detection was developed for the determination of carnosic acid in human plasma and applied to a pharmacokinetic study after oral administration of Rosemary extract to a healthy volunteer. Sample preparation depends on liquid-liquid extraction with hexane. Chromatographic separation was achieved with C18 column (150 mm × 4.6 mm × 5 μm), at 25°C with isocratic elution, mobile phase composed of solution A (methanol), and solution B (2% o-phosphoric acid in water) (90:10, v/v) at flow rate of 1.0 mL/min. The analyte was detected at 230 nm. The retention time is 4.20 ± 0.03 min. The method was validated in terms of accuracy, precision, specificity, robustness and detection and quantification limits, in accordance with European Medicines Agency guidelines. LOD and LOQ were found to be 0.075 and 0.25 ng/mL, respectively. The method was applied to the analysis of carnosic acid in human plasma with good recovery as 91.7%. The plasma concentration-time profile and pharmacokinetic parameters: AUC0-t, AUC0-∞, Cmax, tmax, t1/2 were calculated according to the assays. The method can certainly be used for routine analysis of carnosic acid in human plasma after oral administration of Rosemary extract, and for phase I clinical studies and bioavailability-bioequivalance studies as well.

Two spectrophotometric techniques and a novel HPLC method were consecutively applied for the simultaneous quantification of the active ingredients of emtricitabine (EMC), tenofovir (TNF), and bictegravir (BIC). The first spectrophotometric method is the dual amplitude difference method coupled with the ratio difference method. TNF was determined using the dual amplitude difference method, while BIC and EMC were determined using the ratio difference method. The second spectrophotometric method was the constant multiplication with absorbance extraction method, and was applied for the determination of active substances used in the treatment of human immunodeficiency virus (HIV) infection. BIC was determined by the constant multiplication method, whereas EMC and TNF were determined using the absorbance extraction method. For the HPLC method, the XBridge C18 column was used. The solvent system comprised acetonitrile:phosphate buffer (pH 6.8; 30:70 v/v). All active ingredients were detected at 260.0 nm, and the flow rate was 0.5 mL/min. The experiment was completed within 5.5 min. The experiments carried out enabled the simultaneous analysis of the three active substances and they were economical, fast, environmentally friendly, and simple. The methods have been successfully applied to prepare mixtures and tablets without matrix interference. The methods were evaluated in terms of green chemistry. The methods have been validated according to International Council for Harmonisation (ICH) guidelines.

The present study aims to develop an electroanalytical method to determine one of the most significant antineoplastic agents, topotecan (TPT), using a novel and selective molecular imprinted polymer (MIP) method for the first time. The MIP was synthesized using the electropolymerization method using TPT as a template molecule and pyrrole (Pyr) as the functional monomer on a metal-organic framework decorated with chitosan-stabilized gold nanoparticles (Au-CH@MOF-5). The materials’ morphological and physical characteristics were characterized using various physical techniques. The analytical characteristics of the obtained sensors were examined by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and differential pulse voltammetry (DPV). After all characterizations and optimizing the experimental conditions, MIP-Au-CH@MOF-5 and NIP-Au-CH@MOF-5 were evaluated on the glassy carbon electrode (GCE). MIP-Au-CH@MOF-5/GCE indicated a wide linear response of 0.4–70.0 nM and a low detection limit (LOD) of 0.298 nM. The developed sensor also showed excellent recovery in human plasma and nasal samples with recoveries of 94.41–106.16

Objective: The simultaneous determination of abacavir (ABV), lamivudine (LMV) and zidovudine (ZDV) were applied by dual amplitude difference method coupled with ratio difference spectrophotometric methods. Material and Method: The LMV was quantified by selected the 226.0 nm and 235.0 nm in the dual amplitude difference method. For ratio difference method 297.0 nm and 268.0 nm wavelengths and 266.0 nm, 245 nm wavelengths were chosen to quantify respectively ABV and ZDV. Accuracy studies have been carried out with percent recovery. Result and Discussion: The proposed study, three active substances used in Human immunodeficiency virus (HIV) treatment were quantified. These active ingredients are used in combination to provide effective treatment. With the applied methods, firstly LMV was determined by dual amplitut difference method, then ABV and ZDV were determined by ratio difference. The three active ingredients were studied in the concentration range of 3-21 µg/ml. Correlation coefficients were found to be between 0.9985 and 0.9996. Recovery results range from 95.2 to 106.2. In the method, it was only dissolved in the solvent and measured, and the analysis was carried out without pre-preparation and expensive equipment.

A fast procedure obtained by the combination of fabric phase extraction (FPSE) with high performance liquid chromatography (HPLC) has been developed and validated for the quantification of favipiravir (FVP) in human plasma and breast milk. A sol-gel polycaprolactone-block-polydimethylsiloxane-block-polycaprolactone (sol-gel PCAP-PDMS-PCAP) coated on 100% cellose cotton fabric was selected as the most efficient membrane for FPSE in human plasma and breast milk samples. HPLC-UV analysis were performed using a RP C18 column under isocratic conditions. Under these optimezed settings, the overall chromatographic analysis time was limited to only 5 min without encountering any observable matrix interferences. Following the method validation pro-cedure, the herein assay shows a linear calibration curve over the range of 0.2-50 mu g/mL and 0.5-25 mu g/mL for plasma and breast milk, respectively. The method sensitivities in terms of limit of detection (LOD) and limit of quantification (LOQ), validated in both the matrices, have been found to be 0.06 and 0.2 mu g/mL for plasma and 0.15 and 0.5 mu g/mL for milk, respectively. Intraday and interday precision and trueness, accordingly to the International Guidelines, were validated and were below 3.61% for both the matrices. The herein method was further tested on real samples in order to highlight the applicability and the advantage for therapeutic drug monitoring (TDM) applications. To the best of our knowledge, this is the first validated FPSE-HPLC-UV method in human plasma and breast milk for TDM purposes applied on real samples. The validated method provides fast, simple, cost reduced, and sensitive assay for the direct quantification of favipiravir in real biological matrices, also appliyng a well-known rugged and cheap instrument configuration.