Pharmaceutical Analysis Research Articles

Strategies for the development and optimization of green acetonitrile-free HPLC methods for application in pharmaceutical analysis

Strategies for the development and optimization of green acetonitrile-free HPLC methods for application in pharmaceutical analysis

Design, programming, and evaluation of a serious game web application to memorise drug classification and properties.

Design, programming, and evaluation of a serious game web application to memorise drug classification and properties.

How to proceed with easily recrystallizing secnidazole in designing polyelectrolyte complex-based films for periodontitis treatment?

How to proceed with easily recrystallizing secnidazole in designing polyelectrolyte complex-based films for periodontitis treatment?

Laser-induced graphene electrodes obtained by direct laser writing for pharmaceutical and biomedical analysis

Laser-induced graphene electrodes obtained by direct laser writing for pharmaceutical and biomedical analysis

Recent approaches in green liquid chromatography for pharmaceutical analysis: A comprehensive review on green analytical sustainable chemistry

Recent approaches in green liquid chromatography for pharmaceutical analysis: A comprehensive review on green analytical sustainable chemistry

HPLC and UV Spectroscopy in Pharmaceutical Analysis

Ultraviolet (UV) spectroscopy and High-Performance Liquid Chromatography (HPLC) are two essential analytical methods that are frequently employed in pharmaceutical analysis for regulatory compliance, quality assurance, and medication development. Pharmaceutical substances, such as active pharmaceutical ingredients (APIs), contaminants, and degradation products, can be separated, identified, and quantified using high-performance liquid chromatography (HPLC), a very sensitive and accurate chromatographic technology. It is essential for pharmacokinetic research, stability testing, and bioequivalence evaluations. However, UV spectroscopy is a quick and inexpensive analytical method that helps with both qualitative and quantitative characterization of drug compounds by measuring how much ultraviolet light they absorb. It is widely used for pharmaceutical ingredient concentration determination, dissolving research, and purity testing. For frequent quality checks, UV spectroscopy offers a more straightforward and non-destructive method, even if HPLC gives better selectivity and resolution. Pharmaceutical analysis is more accurate and efficient when these two methods are combined. A popular technique for tracking drug formulations, identifying fake drugs, and guaranteeing batch-to-batch uniformity in production is HPLC combined with UV detection, or HPLC-UV. The concepts, procedures, and comparative uses of HPLC and UV spectroscopy in pharmaceutical analysis are examined in this paper. Their benefits, drawbacks, and most current developments in analytical technology are also covered. Researchers and pharmaceutical experts must be aware of these methods in order to guarantee the safety, effectiveness, and adherence to international regulatory requirements of drugs

Green Electrochemical Sensor for Simultaneous Determination of Linagliptin and Dapagliflozin Using Renewable Carbon Dots

Abstract This study presents a novel electrochemical sensor for simultaneously determining of co-formulated antidiabetic drugs, dapagliflozin (DPG) and linagliptin (LNG) via a carbon paste electrode modified with carbon dots (CDs) prepared from a renewable green source. The carbon dots, derived from avocado peels, were electrodeposited onto the carbon paste to enhance the kinetics of electron transport and the electroactive surface area. Optimization of the electrodeposition parameters is achieved with a limit of detection 3.24 µM, and 2.7 µM, within a range from 1.0×10-5 to 0.36 ×10-3 M and 1.0×10-5 to 0.2×10-3 M for LNG and DPG, respectively. The study highlights the environmental sustainability of a voltammetric electrode, evaluated through green analytical tools like Analytical greenness (AGREE). This approach underscores the potential of green-sourced carbon dots in advancing electroanalytical methods in the field of pharmaceutical analysis.

Utility of unique optical properties of Anethum graveolens green synthesized mediated-alumina nanoparticles for spectrofluorometric determination of darifenacin in pharmaceutical products

In this study, a new fluorescence-based analytical method for the determination of darifenacin (DFN) in pharmaceutical formulations using alumina nanoparticles (NPs) and sodium dodecyl sulfate (SDS) is presented. The alumina NPs were synthesized by a green method using Anethum graveolens (extract as a reducing and stabilizing agent. The NPs were characterized by UV-vis spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FTIR). The method enhanced the fluorescence of alumina NPs in the presence of SDS, which stabilized the particles and maintained their dispersion. DFN interacts with the NPs, enhancing fluorescence emission and allowing sensitive detection at λex/λem (290/400 nm). The method quantifies DFN over a concentration range of 0.1–10 µg/mL, with a limit of detection of 0.013 µg/mL and a limit of quantification of 0.043 µg/mL. The recovery percent is over 99%, which demonstrates the accuracy of the method. In accordance with established methodological guidelines, mean precision was used to accurately assess the precision of the results. This fluorescence-based technique offers several key advantages, including rapid analysis, minimal sample preparation, and high specificity, making it a promising tool for routine quality control and pharmaceutical analysis.

Hyphenated Technique Used for the Analysis of Pharmaceutical Impurities: A Comprehensive Review

The term "Hyphenated Technique" describes a set of analytical techniques that improve pharmaceutical impurity identification and characterization. This comprehensive review uses several hyphenated techniques; The review of hyphenated techniques includes various techniques which are used nowadays for analysis. One of the powerful tools of impurity profile is like Chromatographic techniques like GC, LC etc., which are used for the separation and spectroscopic techniques such as NMR, MS, and IR used for the identification of impurities in pharmaceutical analysis are covered in this thorough overview found as necessary steps to measure for this compounds at extremely low concentrations. Such methods can increase sensitivity, specificity, and resolution, so that patterns of sophisticated impurities in drug substances can be indeed detected. The review would also include issues like regulation as well as challenges in the development of new methods and importance of precise impurity profiling with respect to safety and efficacy in pharmaceuticals. It certainly demonstrates a distinct hyphenated approaches towards modem pharmaceutical quality control and regulatory compliance. Thus, it is in the light of this review that the significance of hyphenated techniques in ensuring drug safety, efficacy and compliance comes out through the current innovations. Nanogram quantities of impurities could otherwise go unnoticed by conventional analytical techniques as hyphenated methods permit their detection. With combined mass spectrometry and chromatography, resolution is improved, high-throughput analysis enhanced, and even trace impurities are quantitated with greater accuracy at concentrations that may be extremely low. These techniques also clarify the impurity structure, which is important in identifying the potential hazards and how it impacts safety and stability with regards to patient care and the drug.

Advanced eco-friendly spectrophotometric analysis for Nebivolol, Valsartan, and related impurity with comprehensive environmental impact assessment

At present, one of the main priorities for analysts is creating more sustainable and environmentally friendly methods for pharmaceutical analysis. In this context, three innovative spectrophotometric techniques, using tri-colored (green, blue, and white), were optimized and developed to simultaneously assess two antihypertensive drugs, Nebivolol hydrochloride (NEB) and Valsartan (VAL), in the presence of synthetic precursor impurity of Valsartan (Valsartan Desvaleryl, VAL-D), which is the main acidic degradation product. The methods employed, including the double divisor-ratio spectra derivative spectrophotometric method, the dual-wavelength in ratio spectrum method, and the H-point derivative ratio method, displayed a good linear range of 2.5–70 µg/mL, 10–50 µg/mL, and 10–70 µg/mL for NEB, VAL, and VAL-D, respectively. Assessment of greenness was implemented to the established methods using the analytical Eco-Scale scoring, analytical greenness metric (AGREE), and the green analytical process index (GAPI). The concepts of blueness assessment using the recently introduced Blue Applicability Grade Index (BAGI tool) and whiteness assessment using the Red Green Blue 12 (RGB 12 tool) were also applied. The proposed methods were validated as per ICH guidelines and verified to be accurate. Statistical analysis was performed to ensure the validity of methods concerning published methods.

SolPred: A machine learning based mobile phase composition prediction tool for the pharmaceutical compounds analysis in RP-HPLC

Artificial intelligence (AI) has gained tremendous growth in chromatography in recent years. Random Forest Classifier (RFC) and Artificial Neural Network models (ANN) were applied to predict the most suitable mobile phase composition for pharmaceutical compounds. To determine the optimal solvent composition for the test compound, RFC was applied to a dataset of molecular descriptors. The RFC utilized the molecular descriptors optimally to select the solvent suitability for the test compounds, while the ANN predicted similar actual and predicted mobile phases in the training set. The model demonstrated high predictive accuracy, with strong correlations for acetonitrile (r = 0.944), methanol (r = 0.961), water (r = 0.983), and buffer (r = 0.918). The model also obtained coefficient of determination (R 2 = 0.902). The ANN model was used to predict the mobile phases of the test compounds. Analytical trials were performed using the predicted mobile phase in isocratic proportion for the test compounds on a C18 column with 1.0 mL/min flowrate. The resulting chromatograms were evaluated to validate the predicted mobile phase. By enhancing the developed method, predictive mobile phase compositions can advance the future of pharmaceutical analysis and serve as a leveraging tool for RP-HPLC analysis.

Characterization of Pharmaceutical Transformation Products by High-Field Asymmetric Waveform Ion Mobility and Infrared Ion Spectroscopy Coupled to Mass Spectrometry.

The identification of drug degradation products is crucial for pharmaceutical development and quality control, as drug transformation products can significantly affect therapeutic efficacy and patient safety. Traditional analytical methods, such as high-performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS), often require reference standards for accurate identification and may be unsuitable for resolving isomeric and isobaric degradation products. This study explores the use of high-field asymmetric waveform ion mobility spectrometry (FAIMS) and infrared multiple photon dissociation (IRMPD) spectroscopy coupled with mass spectrometry (MS) as an effective alternative for identifying drug degradation products without the need for previous chromatographic stages or the use of reference standards. Cyclophosphamide, a widely used DNA-alkylating agent in cancer and autoimmune therapies, is employed as a model system for this study. FAIMS enabled the separation of species based on their differential mobility, while IRMPD provided distinctive spectral data, allowing precise reference-standard-free structural elucidation. This integrated approach offers a robust solution for the identification of complex degradation products, advancing stability studies, formulation development, and quality control in pharmaceutical analysis.

AFM-Based Monitoring of Enzymatic Activity of Individual Molecules of Cytochrome CYP102A1.

Herein, we report the use of a nanotechnology-based approach for the study of enzyme-functionalized mica surfaces. Atomic force microscopy (AFM) has been employed for the determination of the catalytic activity of single molecules of heme-containing cytochrome P450 CYP102A1 (CYP102A1) enzyme, which was immobilized on the surface of a mica chip. Height fluctuations in individual molecules of the enzyme were measured under near-native conditions by AFM measurements in liquid using a cantilever with a 10 to 20 nm tip curvature radius. We have found that in the process of enzymatic catalysis, the mean amplitude of height fluctuations in individual enzyme molecules is 1.4-fold higher than that of enzyme molecules in an inactive state. The temperature dependence of the mean amplitude of height fluctuations in cytochrome CYP102A1 has been revealed, and the maximum of this dependence has been observed at 22 °C. The proposed nanotechnology-based approach can be employed in studies of a wide variety of enzymes, which are important for the development of novel diagnostic tests and systems for pharmaceutical analysis. The approach developed in our work will favor further miniaturization of enzyme-based biosensors and the transition from traditional sensors to nanobiosensors.

Recent Advances and Applications of Green Analytical Chemistry in Environmental Monitoring, Food Safety, and Pharmaceutical Analysis

Abstract: Green analytical chemistry (GAC), which emphasizes environmental sustainability and responsibility, has now become an attractive choice for researchers. This review article provides a comprehensive introduction to the principles of GAC, which involve reducing excessive solvent consumption, toxicity of reagents, high power output, and complex sample treatment, making the analytical processes more efficient and effective. The article also highlights the recent developments in analytical techniques, like microfluidic devices [miniaturized extraction methods (combining LPME with DES, QuEChERS)], greenness evaluating tools (GAPI, AGREE, NEMI, Eco-scale, etc.) for data analysis, as well as metal-organic frameworks (like bimetallic MoF, Zn-MoF, etc.) to enhance detection sensitivity and specificity due to their larger surface area and superior physical properties as compared to traditional sorbents. Furthermore, these innovations are essential to meet the growing demand for less expensive and more environment-friendly methods for analysis. The various applications of GAC in the fields of food safety, environmental monitoring, and pharmaceutical analysis are discussed here, which might lead to a revolution in analytical techniques, improving health outcomes and fostering environmentally friendly societies.

Evaluating Artificial Intelligence Tools in the Pharmaceutical Industry: A Case Study on Paracetamol Dissolution and Calibration Curves

Purpose: This study evaluates the potential of artificial intelligence (AI), specifically ChatGPT, in assisting with the analysis of paracetamol dissolution tests and the construction of calibration curves. The primary research question investigates whether AI-generated data can approximate real laboratory results for pharmaceutical quality control, with an emphasis on exploring the limitations and applications of AI in pharmaceutical analysis. Methods: Paracetamol solutions were prepared, and their absorbance was measured using a UV-Vis spectrophotometer to construct calibration curves. Dissolution tests were performed in phosphate buffer solution, and both real and AI-generated data were analyzed. ChatGPT generated hypothetical data for the calibration curves and dissolution profiles, which were then compared to actual laboratory results. Statistical methods such as mean squared error (MSE), percent error, and correlation coefficients (R²) were employed to evaluate the accuracy of the AI-generated data. A paired t-test was used to determine the statistical significance of differences between the datasets. Results: AI-generated data followed general trends in both the calibration curve and dissolution tests but exhibited significant discrepancies in accuracy. Absorbance values from the AI model were consistently lower than real measurements, while AI overestimated drug release in early dissolution stages. The MSE for dissolution tests was 47.80, while for calibration curves, it was 0.0583. Despite these differences, AI-generated data aligned more closely with real data at later dissolution time points. Conclusions: While AI tools like ChatGPT can approximate trends in pharmaceutical analysis, real laboratory data are essential for accuracy, particularly in the early stages of testing. AI shows potential as a supplementary tool for theoretical understanding but cannot replace hands-on experimentation.

A NOVEL REVERSE-PHASE ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD WITH GRADIENT ELUTION FOR SIMULTANEOUS DETERMINATION OF DOLUTEGRAVIR, LAMIVUDINE AND TENOFOVIR DISOPROXIL FUMARATE IN FIXED-DOSE COMBINATION

ABSTRACT Objective: To develop a sensitive and rapid reverse phase ultra-performance liquid chromatographic method for the simultaneous determination of dolutegravir (DTG), lamivudine (LAM), and tenofovir disoproxil fumarate (TDF) with improved separation and stability-indicating features. Methods: Chromatographic separation was performed on an acquity bridged ethyl siloxane/silica hybrid C18 (50 × 2.1 mm, 1.7 μm) column at 40°C using 0.05% trifluoroacetic acid in water (pH 3.0) and methanol as mobile phase, with a flow rate of 0.4 mL/min and ultraviolet detection at 265 nm. The method validation was performed per ICH guidelines and included stress degradation studies. Results: Effective separation was achieved; retention times were 1.25 min for LAM, 2.87 min for TDF, and 3.65 min for DTG. Supporting validation, the limits of linearity were set at 15–90 μg/mL for both LAM and tenofovir, and 2.5–15 μg/mL for DTG, with R2 values exceeding 0.999. Conclusion: The proposed technique provides high accuracy, precision, sensitivity, and specificity in detecting multiple antiretroviral drugs in fixed-dose drug combinations. Compared to previously published methods, the gradient elution profile offers better peak height, greater peak splitting, as well as decreased total time required for analysis. The method’s stability-indicating features, confirmed by forced degradation studies, demonstrate the method’s value for pharmaceutical analysis quality control and stability testing.

Click chemistry in drug development recent trends and application

K. Barry Sharpless invented click chemistry in 2001, and it has revolutionized drug development with its effective, diverse, and selective chemical synthesis. In fact, the copper(I)-catalyzed azide-alkyne cycloaddition (CuAAC) process has become a crucial tool for drug-like particle assembly, functionalization of physiologically active mixtures, and accurate drug-biomolecule conjugation. Late-stage click chemistry applications span a number of industries, including prodrugs, antibody-drug conjugates (ADCs), and specific drug delivery systems including hydrogels and nanoparticles. Click reactions' high specificity and bio-orthogonality have increased therapeutic precision, lessening side effects and improving therapeutic outcomes. New reactions, such as sulfur-fluoride exchange (SuFEx) and strain-promoted azide-alkyne cycloaddition (SPAAC), are a part of emerging trends in click chemistry that expand the range of applications. Click chemistry has improved lead compound synthesis, made it easier to develop pharmacophore linkers, and produced bio isosteres to improve drug potency and metabolic stability in the drug discovery process. The method's role in creating cutting-edge treatments has also been highlighted by its contribution to the discovery of inhibitors for diseases like HIV, cancerous development, and bacterial infections. From early stage drug discovery to clinical development, click chemistry remains at the forefront of pharmaceutical analysis, highlighting its critical influence on ongoing drug development.

Electrochemical Determination of Acetaminophen and Amoxicillin Using CuO/Graphitic Carbon Nitride Hybrid Composite Modified Electrode

Abstract Acetaminophen (PCM) and amoxicillin (AMX) are commonly used drugs, but their overuse and environmental release pose risks to human health and ecosystems. A simple sensor based on a 2D hybrid composite of copper oxide and graphitic carbon nitride (CuO/GCN) was developed to detect PCM and AMX. The CuO/GCN sensor was synthesized using hydrothermal and sonochemical methods and characterized by UV-visible spectroscopy, Fourier transform infrared spectroscopy, high-resolution scanning electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction. Electrochemical detection was performed with cyclic voltammetry and amperometric techniques. The sensor showed high sensitivity with detection limits of 6.8 nM for PCM and 12.9 nM for AMX, with broad linear ranges of 0.025–939.15 µM for PCM and 0.025–8.55 µM for AMX in PBS at pH 7.4. It demonstrated excellent repeatability, reproducibility, and selectivity. The sensor was successfully applied to tap water and human urine, showing high recovery rates of 100.7–100.4% for PCM and 102.0–104.7% for AMX. This CuO/GCN sensor shows potential for pharmaceutical analysis and environmental monitoring.

Comparative Quantitative Study of Acetyl Salicylic Acid in Aspirin Samples Using Spectrophotometry and Volumetric

This study focuses on the quantification of acetylsalicylic acid (ASA) in aspirin tablets using two analytical approaches: back-titration and spectrophotometric analysis. Significant variations in ASA concentrations were observed across different samples. The back-titration method recorded concentrations ranging from 33.68% to 75.27%, while spectrophotometric analysis yielded values between 26.27% and 74.65%. These discrepancies highlight potential factors such as formulation inconsistencies, manufacturing quality, or chemical interactions during analysis. A comparative evaluation of the two methods reveals that the spectrophotometric method demonstrated higher precision and ease of execution, making it suitable for routine pharmaceutical analysis. However, both methods showed limitations in accuracy. The findings suggest variability in ASA concentrations among different commercial brands, which remain largely within official standards but warrant further investigation to ensure consistency and efficacy. The study underscores the need for refining analytical methods to enhance reliability and calls for improved manufacturing protocols to maintain quality control in pharmaceutical products.

Cobalt oxide modified screen-printed carbon electrode for electrochemical detection of high blood pressure treating drug: reserpine.

This study presents the development of a cobalt oxide-modified screen-printed carbon electrode (CoO/SPCE) for the electrochemical detection of reserpine (RES), a drug used to treat high blood pressure. The CoO/SPCE was fabricated using an optimized electrodeposition method, resulting in a sensitive and reproducible platform for RES detection. Electrochemical characterization demonstrated that the CoO/SPCE exhibited superior electrocatalytic activity, as evidenced by a notable increase in oxidation peak current compared to bare and activated SPCEs. The electrode showed a linear response to RES concentrations ranging from 2 to 100μM with a detection limit of 1.08μM. Additionally, the sensor demonstrated good stability and reproducibility with relative standard deviations (RSDs) of 5.11% and 2.72%, respectively. This work highlights the CoO/SPCE's potential for practical pharmaceutical analysis, offering a novel approach to enhancing the sensitivity and reliability of electrochemical sensors for drug monitoring.