Pharmaceutical Quality Control Research Articles

AIE-based fluorescent sensing of ciprofloxacin using non-fluorescent 2D silver dimolybdate nanosheets: The synergistic sensor method (SGSM) to switch on non-fluorescent 2D nanosheets into an effective fluorescent biosensor

The development of an efficient method for detecting ciprofloxacin (CIP) is critical due to the potential for significant harm to humans, including the danger of severe liver damage and hematuria associated with increased levels of this drug. In this study, we offer a highly sensitive and highly selective method for fluorescence sensing of the antibiotic ciprofloxacin employing the properties of Aggregation-Induced Emission (AIE) with silver dimolybdate nanosheets (Ag2Mo2O7 NSs). Outstanding structural characteristics of the Ag2Mo2O7 NSs achieved using the hydrothermal method. By carefully controlling the aggregation of the Synergistic Sensor Method (SGSM), we are able to produce a very bright fluorescence response with the ciprofloxacin concentration range from 0 to 250 nM with a low detection limit of 1.1 nM. Quick and ultrasensitive detection has been achieved by the Synergistic effect (SGE) and AIE from the current approach. The SGSM has been shown to be a novel platform for human health monitoring and pharmaceutical quality control. With broad-ranging practical implications, the combination of AIE and silver dimolybdate nanosheets offers a platform for reliable and ciprofloxacin detection. We believe the SGSM is a role model paper for future nano-biosensor detection methods due to the synergistic effect resulting in the AIE and turn-on sensor approach for many non-fluorescent 2D nanosheets. This can open many new doors for the intensive development of 2D nanosheets for future fluorescent sensors without the need to produce fluorescence by the nanosheet itself.

UV imaging for the rapid at-line content determination of different colourless APIs in their tablets with artificial neural networks

This paper presents a novel high-resolution and rapid (50 ms) UV imaging system, which was used for at-line, non-destructive API content determination of tablets. For the experiments, amlodipine and valsartan were selected as two colourless APIs with different UV induced fluorescent properties according to the measured solid fluorescent spectra. Images were captured with a LED-based UV illumination (385–395 nm) of tablets containing amlodipine or valsartan and common tableting excipients. Blue or green colour components from the RGB colour space were extracted from the images and used as an input dataset to execute API content prediction with artificial neural networks. The traditional destructive, solution-based transmission UV measurement was applied as reference method. After the optimization of the number of hidden layer neurons it was found that the relative error of the content prediction was 4.41 % and 3.98 % in the case of amlodipine and valsartan containing tablets respectively. The results open the possibility to use the proposed UV imaging-based system as a rapid, in-line tool for 100 % API content screening in order to greatly improve pharmaceutical quality control and process understanding.

Impressive spectrofluorimetric framework for determination of newly approved anti-coagulant betrixaban using silver-nanoparticles; with assessment of blueness, whiteness and greenness.

A straight-forward, affordable, sensitive and ecologically friendly spectrofluorimetric method was introduced for the determination of the newly approved direct oral anticoagulant drug betrixaban (BXN) at the nano-scale level. The approach is based on turning on the fluorescence of BXN using silver nanoparticles (AgNPs). The synthesis of silver nanoparticles was based on the reduction capability of BXN in response to silver nitrate using polyvinylpyrrolidone (PVP) as a stabilizing agent, and sodium hydroxide solution for promoting the continuity of the nucleation and growth processes of AgNPs. The synthesized AgNPs were recognized and characterized using UV/visible spectroscopy, Transmission Electron Microscope (TEM), Zeta Potential, Dynamic Light Scattering (DLS) and Fourier Transform Infrared Spectroscopy (FTIR). The fabricated AgNPs were found to enhance the fluorescence intensity of BXN, allowing its sensitive and precise quantitative determination at an emission wavelength of 369 nm after excitation at 303 nm. The proposed approach, verified in compliance with International Conference on Harmonization (ICH) guidelines, achieved linearity over a concentration range of 0.20–1.5 μg/mL with quantification and detection limits of 0.097 and 0.032 μg/mL, respectively. BXN was estimated in its pure form with a high percentage recovery of 100.52 % and a correlation coefficient of 0.9997. The studied approach was successfully applied for the assay of BXN in newly approved pharmaceutical dosage form with a high percentage of recovery (%Recovery = 100.20 %) and a low percentage of error (%Error = 0.96). Integration of white analytical chemistry was our emphasis in this study to provide sustainable analytical insight. Blueness (BAGI), whiteness (RGB Algorithm) and greenness (GABI and AGREE) of the evolved method were evaluated. An excellent white and green profile with satisfactory results and scores indicated the sustainability and impressive applicability of the evolved approach in pharmaceutical companies and quality control laboratories.

Validation, measurement uncertainty estimation and evaluation of UHPLC greenness for simultaneous determination of metoprolol tartrate and hydrochlorothiazide in binary tablet

A novel green ultra high performance liquid chromatography (UHPLC) method was validated and estimated the measurement uncertainty for simultaneous determination of metoprolol tartrate (MET) and hydrochlorothiazide (HCT) in binary tablet. A Zorbax® SB-C18 column with isocratic elution (flow rate 0.9 mL min−1) at 25°C was used. Analytes and HCT degradation product were separated in approximately 1 min using acetonitrile:water:triethylamine (17:83:0.2, v/v) as mobile phase. Analytical curves were linear with (R 2 > 0.99 for MET and HCT) with detection limits of 2.42 and 1.05 µg mL−1 for MET and HCT, respectively. Precision measurements showed RSD% from 0.39 to 1.2% and method accuracy by recovery tests was 100 ± 2%. Measurement uncertainties using Eurachem procedure were 100.1 ± 2.8% and 100.3 ± 2.4% for MET and HCT, respectively. This UHPLC method was accurate, precise, linear and selective, making it suitable for pharmaceutical quality control. It also proved eco-friendly compared to other reported methods.

Carbon dots-adorned silver nanoparticles as a straightforward sustainable colorimetric sensor for the rapid detection of ketotifen in eye drops and aqueous humor

The rapid and accurate detection of drug molecules in pharmaceutical formulations and biological samples is of paramount importance. In this research article, we present a novel colorimetric sensor based on carbon dots decorated silver nanoparticles (CDs/AgNPs) for the rapid detection of ketotifen (KTF), a widely used antihistamine drug. The CDs were synthesized via a facile one-step microwave-assisted method and subsequently conjugated onto AgNPs through a simple adsorption process, forming a stable CDs/AgNPs composite. The resulting composite exhibited unique optical properties, including a strong absorption peak at 410 nm with remarkable intensity reduction and color changes upon the addition of KTF. The developed colorimetric sensor exhibited a wide linear range of 3.0–40.0 µg mL−1 (R2 = 0.9996), with a %RSD of 2.41, and a low limit of detection (LOD) of 0.981 µg mL−1. Furthermore, the sensor's practical applicability was evaluated by successfully detecting KTF in eye drops and artificial aqueous humor, demonstrating a remarkable percentage recovery exceeding 96.0 %. Finally, a comprehensive evaluation of the greenness and blueness of the method was performed using analytical eco-scale, GAPI, AGREEprep, and BAGI tools. The results of these assessments indicate its exceptional sustainability. Overall, the proposed method holds significant potential for applications in pharmaceutical quality control and therapeutic monitoring, contributing to improved patient care and drug safety in the field of ophthalmology.

Four chemometric models enhanced by Latin hypercube sampling design for quantification of anti-COVID drugs: sustainability profiling through multiple greenness, carbon footprint, blueness, and whiteness metrics

Montelukast sodium (MLK) and Levocetirizine dihydrochloride (LCZ) are widely prescribed medications with promising therapeutic potential against COVID-19. However, existing analytical methods for their quantification are unsustainable, relying on toxic solvents and expensive instrumentation. Herein, we pioneer a green, cost-effective chemometrics approach for MLK and LCZ analysis using UV spectroscopy and intelligent multivariate calibration. Following a multilevel multifactor experimental design, UV spectral data was acquired for 25 synthetic mixtures and modeled via classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), and genetic algorithm-PLS (GA-PLS) techniques. Latin hypercube sampling (LHS) strategically constructed an optimal validation set of 13 mixtures for unbiased predictive performance assessment. Following optimization of the models regarding latent variables (LVs) and wavelength region, the optimum root mean square error of cross-validation (RMSECV) was attained at 2 LVs for the 210–400 nm spectral range (191 data points). The GA-PLS model demonstrated superb accuracy, with recovery percentages (R%) from 98 to 102% for both analytes, and root mean square error of calibration (RMSEC) and prediction (RMSEP) of (0.0943, 0.1872) and (0.1926, 0.1779) for MLK and LCZ, respectively, as well bias-corrected mean square error of prediction (BCMSEP) of -0.0029 and 0.0176, relative root mean square error of prediction (RRMSEP) reaching 0.7516 and 0.6585, and limits of detection (LOD) reaching 0.0813 and 0.2273 for MLK and LCZ respectively. Practical pharmaceutical sample analysis was successfully confirmed via standard additions. We further conducted pioneering multidimensional sustainability evaluations using state-of-the-art greenness, blueness, and whiteness tools. The method demonstrated favorable environmental metrics across all assessment tools. The obtained Green National Environmental Method Index (NEMI), and Complementary Green Analytical Procedure Index (ComplexGAPI) quadrants affirmed green analytical principles. Additionally, the method had a high Analytical Greenness Metric (AGREE) score (0.90) and a low carbon footprint (0.021), indicating environmental friendliness. We also applied blueness and whiteness assessments using the high Blue Applicability Grade Index (BAGI) and Red–Green–Blue 12 (RGB 12) algorithms. The high BAGI (90) and RGB 12 (90.8) scores confirmed the method's strong applicability, cost-effectiveness, and sustainability. This work puts forward an optimal, economically viable green chemistry paradigm for pharmaceutical quality control aligned with sustainable development goals.

Development of a technique for determining the viability of dormant organisms in powdered substances

The purposes of pharmaceutical biotechnology and quality control of probiotics containing lyophilized bacterial preparations, as well as the purpose of ensuring biological safety, require methods for rapid determination of the viability of dormant forms. This paper describes an approach to determining the viability of dry powdered substances. Lyophilized powder of Kalanchoe daigermontiana, dry dormant eggs of Artemia salina, and dry powder of Lycopodium sp. spores were proposed as model objects. Suspensions of virus-like particles (VLPs) to SARS-CoV-2 were proposed as a cell-free reference material. The following methods of elemental analysis were used in the study: X-ray fluorescence spectroscopy (XRF) on an energy-dispersive device, atomic absorption spectroscopy with electrothermal atomization, and Zeeman background correction (GZ-AAS). The free water content was determined by NMR spin echo. A new method was also used for recording the kinetics of changes in broadband radio emission in the centimeter and millimeter wavelength ranges, with a measurement duration of up to 20 minutes. Live and inactivated powdered preparations of K. daigermontiana and A. salina were prepared and characterized by elemental composition, water content, and spin-spin relaxation time (T2). For these live and inactivated preparations, it was determined that the flux density of intrinsic thermal radio emission decreases by an order of magnitude with the loss of viability. In the future, the results obtained will allow for a rapid test of the viability of lyophilized therapeutics (from medicinal plants to bacterial mixtures that stabilize the intestinal microflora).
 Keywords: millimeter emission, X-ray fluorescence analysis, NMR spin echo, nanoparticles, powdered substances, medicinal plant raw materials

Development and Validation of a New Reversed Phase HPLC Method for the Quantitation of Azithromycin and Rifampicin in a Capsule Formulation.

This research aimed to develop a new method for simultaneously estimating the presence of azithromycin (AZT) and rifampicin (RIF) in a capsule formulation using reverse-phase high-performance liquid chromatography. The developed method utilized a Gemini column with a 60:40% v/v acetonitrile and potassium dihydrogen phosphate mobile phase, a flow rate of 1mL/min, and an injection volume of 20μL. The detection wavelengths of 210 and 254nm for AZT and RIF, respectively, were used. Validation ensures specificity with a peak purity index > 0.99999 for AZT and >0.99995 for RIF, affirming unambiguous analyte detection. The system suitability test, within acceptable limits, validates method reliability. Linearity calibration curves (R2 = 0.998) cover a 25-150% target concentration range. Accuracy studies employing the standard addition method yield recovery values between 96.6 and 103.9% for both drugs, confirming method accuracy. Precision studies reveal % relative standard deviation values consistently below 2%, highlighting reproducibility. Robustness testing supports method reliability under varying conditions. Application to a pharmaceutical capsule formulation demonstrates the method's practicality, accurately quantifying AZT (98.30%) and RIF (99.37%). This study provides a validated analytical approach for simultaneous quantification in commercial pharmaceutical products containing both drugs, enhancing pharmaceutical quality control for critical antibiotics in complex formulations.

Comprehensive analysis of vitamin D3 impurities in oily drug products using supercritical fluid chromatography-mass spectrometry.

Vitamin D3 , an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D3 and five non-esters including four that are isobaric to vitamin D3 . Firstly, a screening study highlighted the Torus 1-AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions. Secondly, make-up solvent composition and MS settings were optimized to reach high sensitivity. For both the separation and MS response, the screening design of experiments proved useful. Lastly, a fast saponification and liquid-liquid extraction method was developed, enabling efficient sample cleanup and impurities recovery from the complex oily matrix. The SFC-MS method suitability was assessed in two validation studies. The first study employed the ICH Q2 guideline for impurity limit test to demonstrate method specificity and establish a limit of detection (LOD) and a limit of quantification (LOQ) at 0.2% and 0.5%, respectively, for ester impurities. The second study conducted a comprehensive quantitative assessment for three non-ester impurities using a total error approach, determining method validity through accuracy profiles. The validated method exhibited reliable performance across impurity concentrations from 0.1% to 2.0%, with estimated LODs ranging from 2 to 7ng/mL. This study further promotes SFC-MS as a valuable, versatile, and green tool for routine pharmaceutical QC.

Whiteness and greenness appraisal approaches for quantitative determination of recently approved combination of indacaterol and mometasone via utilization of nuclear magnetic resonance technique

Quantitative proton nuclear magnetic resonance (1H-qNMR) is currently being used in a variety of applications in many disciplines due to the great privileges. Economical and minimal solvent system volume is utilized; no sample labelling or pre-treatment is necessary. Furthermore, no sample destruction is occurred. The all aforementioned benefits are contributed to its suitability for employment in pharmaceutical companies and quality control laboratories. Starting from this significance, a simple, quick, and sustainable method was developed for the determination of indacaterol (IND) and mometasone (MOM) in the raw material and newly approved pharmaceutical dosage form Atectura Breezhaler®. The developed approach involved the utility of pyridoxine (PYR) as an internal standard (IS) and DMSO-d6 as the suitable deuterated solvent for the analysis. The quantitative peaks of IND (doublet at 8.247 and 8.254 ppm) and MOM (singlet at 1.014 ppm) were obviously disengaged from the IS peak; which was singlet peak at 8.082 ppm. The developed methodology was perfectly linear over concentration range of 0.05–5.00 and 0.001–1.00 mg/mL for IND and MOM, respectively. The developed protocol was applied successfully for the determination of IND and MOM mixtures, including capsule-based inhaler dosage form with % recovery of 100.15% and 97.98% for IND and MOM, respectively. Also, the greenness and whiteness (GAPI, AGREE and RGB-algorithm approaches) of the evolved method were evaluated in order to assess its impacts on the ecosystem. The method was proved to possess ecofriendly properties without any expected harmful effects on the environment.

Multivariate statistical approach in food and pharmaceutical quality control

IR spectra contain chemical information of matter and can be acquired from raw/untreated samples. The spectra are, however, complicated to interpret and could not be used directly for both qualitative and quantitative purposes. In this research a statistical approach namely, multivariate data analysis (MVDA) or chemometrics was employed for mining information related to chemical compositions from spectroscopic data. Two examples are used to illustrate the potential of this approach, one is edible oil (using benchtop FT-IR), and pharmaceuticals (using handheld NIR). Olive oil was differentiated from adulterants (sesame, sunflower, palm oil) in PCA, and the content of olive oil was successfully determined by the PLS model the error of olive oil content < 5%. Norfloxacin content in lab-scale powder formulation yield the auspicious results with the error < 6%. The results proved the developed techniques are promising for rapid analysis at significantly lower costs.

Advancing drug safety and mitigating health concerns: High-resolution mass spectrometry in the levothyroxine case study

Levothyroxine is a drug with a narrow therapeutic index. Changing the drug formulation composition or switching between pharmaceutical brands can alter the bioavailability, which can result in major health problems. However, the increased adverse drug reactions have not been fully explained scientifically yet and a thorough investigation of the formulations is needed.In this study, we used a non-targeted analytical approach to examine the various levothyroxine formulas in detail and to reveal possible chemical changes. Ultra-high-performance liquid chromatography coupled with a data-independent acquisition high-resolution mass spectrometry (UHPLC-DIA-HRMS) was employed.UHPLC-DIA-HRMS allowed aside the detection of levothyroxine degradation products also the presence of non-expected components in the formulations. Among these, we identified compounds resulting from reactions between mannitol and other excipients, such as citric acid, stearate, and palmitate, or from reactions between an excipient and an active pharmaceutical ingredient, such as levothyroxine-lactose adduct. In addition to these compounds, undeclared phospholipids were also found in three formulations. This non-targeted approach is not common in pharmaceutical quality control analysis. Revealing the presence of unexpected compounds in drug formulations proved that the current control mechanisms do not have to cover the full complexity of pharmaceutical formulations necessarily.

Certification of a pharmacopoeial reference standard for potency testing of recombinant interferon α-2b

SCIENTIFIC RELEVANCE. Potency testing of recombinant interferons requires a reference standard. The availability of International Standards (ISs) that are commonly used to assess the quality of recombinant interferons is currently limited. Therefore, the quality of interferons should be assessed using pharmacopoeial reference standards (RSs) certified using ISs (if available).AIM. This study aimed to certify a pharmacopoeial RS for potency testing of recombinant interferon α-2b.MATERIALS AND METHODS. The potency determination involved comparing the inhibition of the virus-induced cytopathic effect observed in cell culture with the candidate RS and the WHO International Standard for Human rDNA-derived interferon α-2b. The study used A-549 and MDBK cell lines with encephalomyocarditis (EMC) and vesicular stomatitis (VSV) viruses. The authors followed the requirements of the State Pharmacopoeia of the Russian Federation (Cell-Culture Bioassays for Interferon Products, OFS.1.7.2.0002.15). The results were recorded using instrumental and visual methods. The calculations used mathematical statistics. To factor in the influence of intermediate precision, the authors applied Student’s t-test.RESULTS. The authors developed a certification programme and procedure and certified the pharmacopoeial RS for recombinant human interferon α-2b (rhIFN α-2b) to identify the corresponding medicinal products (by virus neutralisation) and test their potency (by antiviral activity in cell culture). Upon receipt, the candidate RS was verified for compliance with regulatory specifications. According to the test results, the potency of the candidate pharmacopoeial RS was 4.47×108 IU/mL, and the expanded uncertainty was 8.12×107 IU/mL, with a coverage factor of k=2 and a confidence level of 95%. The pharmacopoeial RS for rhIFN α-2b was considered to have the same shelf-life period as the corresponding medicinal products if stored at a temperature not higher than –40 ºC. When thawed, the pharmacopoeial RS for rhIFN α-2b can be stored at a temperature of 2–8 ºC for up to 1 month.CONCLUSIONS. Upon certification for potency testing, the pharmacopoeial RS for rhIFN α-2b has been included in the Register of Reference Standards of the Russian Pharmacopoeia as Recombinant Human Interferon α-2b (Potency) FSO.3.2.00455. The introduction of this pharmacopoeial RS will help to conduct the identification and potency testing of all Russian interferon α-2b products at an appropriate scientific and methodological level. As a result, Russian pharmaceutical manufacturers and quality control agencies will no longer depend on imported ISs.

ИСПОЛЬЗОВАНИЕ УФ-СПЕКТРОФОТОМЕТРИИ В АНАЛИЗЕ И СТАНДАРТИЗАЦИИ СУБСТАНЦИИ 2-БЕНЗОИЛАМИНО-N-[4-(4,6-ДИМЕТИЛПИРИМИДИН-2-ИЛСУЛЬФАМОИЛ)-ФЕНИЛ]-БЕНЗАМИДА

Borderline neuropsychiatric disorders firmly hold a leading position in a large group of mental illnesses, among which neuroses occupy a significant place. The increasing number of patients with diseases associated with neuropsychiatric disorders makes the search and introduction of highly effective anxiolytics and antidepressants into medical practice increasingly important. In parallel with the search for medicinal substances with such pharmacological properties, it is necessary to resolve issues of standardization and quality control. One of these drugs may be a new synthetic derivative of ortho-benzoylaminobenzoic acid, which has antidepressant and anxiolytic effects. This compound was synthesized at the department of organic chemistry of the Pyatigorsk Medical and Pharmaceutical Institute under the leadership of professor Kodonidi I.P. Several biologically active compounds were synthesized - derivatives of o-benzoylaminobenzoic acid, one of which is 2-benzoylamino-N-[4-(4,6-dimethylpyrimidin-2-ylsulfamoyl)-phenyl]-benzamide (laboratory code - PMFI-195) . Preliminary pharmacological studies of PMFI-195, carried out on the basis of the Federal State Budgetary Educational Institution of Higher Education of the Stavropol State Medical University of the Ministry of Health of Russia and the Federal State Budgetary Educational Institution of Higher Education of the North Caucasus Federal University, under the leadership of professor Manvelyan E.A., showed the promise of developing a drug based on the substance PMFI-195 for the treatment of such diseases such as depression, neuroses, psychopathy, neurosis-like and psycho-like states. Quality control and development of modern methods of pharmaceutical analysis is one of the basic stages of introducing pharmaceutical substances into production. This requires an in-depth study of physicochemical characteristics, as well as the selection and justification of methods of analysis and quality control of pharmaceuticals. substances. The results of the developed method for the qualitative determination by UV spectrophotometric method of a new quinosalinone derivative 2-benzoylamino-N-[4-(4,6-dimethylpyrimidin-2-ylsulfamoyl)-phenyl]-benzamide, which has anxiolytic and antidepressant activity, are presented.

Quality Control and Phytochemical Profiling of a Polyherbal Traditional Indian Medicine by GC-MS method

Introduction: Gomutra (Cow's urine) has been described to be the most effective substance of animal origin. It is useful in treating various diseases due to its pharmacological activities. Nevertheless, due to its pungent smell, palatability, shelf life and fresh availability have always remained a problem. So it is very much essential to modify it into different dosage forms. One of its traditional dosage forms is Gomutrasava, an alcoholic fermented product indicated in the management of Shvitra (vitiligo). Aim & objective: The study is planned for Pharmaceutical preparation and quality control assessment of Gomutrasava. Material & Methods: Gomutrasava was prepared according to a reference from Astanga Hrudaya. This formulation was tested for organoleptic characters and physicochemical parameters, including Gas Chromatography-Mass Spectrometry (GC-MS). Observation & Results: After fermentation colour of Gomutrasava appeared dark brown with specific cow urine smell. pH, specific gravity at 25ºC, reftractive index, brix, viscocity, total solid content, alcohol content, reducing sugar, non reducing sugar of Gomutrasava were 5.41, 0.967 wt/ml, 1.394, 37º, 1.38/sec, 37%, 6%, 0.96%, 0.07% respectively and test for methanol and microbial contamination were negative. GC-MS revealed some compounds attributed to antimicrobial, anticancerous and antifungal activities. Conclusion Thus this data combined with analytical data will be used for clinical study and treatment of Shvitra (Vitiligo), Kushtha (Leprosy) and various skin diseases.

Voltammetric methods for electrochemical characterization and quantification of artemether-based antimalarials.

Every year substandard and falsified (SF) artemisinin derivative-based antimalarials are responsible for the loss of 450 000 deaths and billions of GBP. The lack of infrastructure and funds to support pharmaceutical quality control in many low-and-middle-income countries contributes to this problem. This work assesses fitness for purpose of voltammetric methods for identification and quantification of artemether in the presence of excipients. Electrochemical characterization of artemether using cyclic voltammetry shows that the reduction of artemether is chemically irreversible within the potential range of -0.4 V to -1.4 V. A chronocoulometric quantification algorithm for artemether is created and tested with pure artemether, as well as filtered and unfiltered Riamet® tablets. Filtration of Riamet® tablets provides no additional benefit for the quantification of artemether in Riamet®. In addition, artemether's response to pH indicates possible protonation and coupled homogeneous chemistry. Finally, sodium sulfite is an effective means of removing dissolved oxygen and improving artemether signal resolution in air-equilibrated PBS. This concludes that electrochemical analysis is a promising method for artemether identification and quantification.

Development and Validation of Dissolution Test Method for Herbal Medicine Containing Ginsenosides

Background and objective: This study aimed to develop a dissolution test method for quality control of commercial 40% ethanol extract of ginseng-containing dosage forms.Methods: Through preliminary dissolution testing of the commercial dosage forms, suitable parameters for HPLC (high performance liquid chromatography) analysis were determined, including an injection volume of 50 μL and a dissolution time of 1 hour. Additionally, the stability testing of the solution enabled the selection of an appropriate dissolution medium, pH 4.0 buffer solution. Method validation was carried out using reference standard of eight ginsenosides (Rg1, Re, Rf, Rg2, Rb1, RC, Rb2, Rd), indicative components of ginseng, under the selected testing conditions. The evaluation of method validation encompassed specificity, accuracy, precision, and linearity as assessment criteria.Results: The accuracy assessment revealed that the average recovery rates within a 95% confidence interval were appropriate for all ginsenosides, ranging from 98.25% to 101.17%. The precision evaluation, conducted at an intermediate concentration of 8 μg/mL (n = 6), demonstrated relative standard deviations of 0.25% to 1.08%, which met the criterion of being below 2%. The linearity assessment showed that the coefficient of determination (R²) values for all ginsenosides exceeded 0.999, indicating excellent linearity. The quantification limits ranged from 0.32 to 1.09 μg/mL, confirming their suitability for dissolution assessment of the respective formulation. Employing the selected dissolution test method, the dissolution profiles of most ginsenosides in the commercially available ginseng-containing dosage forms reached their maximum values within 60 minutes. No significant differences were observed in results beyond 120 minutes, confirming that a dissolution time of 60 minutes is appropriate for this dosage form.Conclusion: The established method holds promise as a valuable tool for quality control of pharmaceuticals containing ginseng, including those previously unassessed, contributing to future applications in the pharmaceutical industry.

A Green Raman Spectroscopic Assay Method for The Quantification of Tranexamic Acid in Pharmaceutical Formulations

Tranexamic acid (TXA) is a widely used antifibrinolytic agent that is used to prevent and treat excessive bleeding. Current analytical methods for TXA are often time-consuming and require the use of toxic solvents. Raman spectroscopy has the ability to measure TXA because it is a fast and non-destructive analytical method. This research established and validated a green Raman spectroscopic test for TXA measurement. There was no need for harmful solvents because the technique relied on a basic aqueous solution of TXA. Results demonstrated that the technique was linear across the 0.7% to 13.0% concentration range. The method was also shown to be accurate, with results comparable to the orthogonal techniques. The green Raman spectroscopic assay method was applied to the quantification of TXA in pharmaceutical formulations. The results obtained were comparable to those obtained using reference methods. To quantify TXA quickly and accurately, one can use the green Raman spectroscopic test. Since no harmful chemicals are needed for the procedure, it is also eco-friendly. Method has the potential to be used in a variety of settings, including pharmaceutical quality control and research laboratories.

Deciphering the role of Andrographis paniculata in pharmaceutical field and chromatographic evaluation of Andrographis paniculata in the solution of methanol and hexane through HPTLC

This article explores the medicinal potential of Andrographis paniculata (Kalmegh) in Ayurveda, focusing on its hepato protective and anti febrile properties. The paper emphasizes the importance of herbal medicines in primary health care due to their availability, compatibility, and affordability. Additionally, it discusses the rich herbal medicinal wealth in India and the historical significance of Ayurveda. The study delves into the pharmacological actions of Andrographis paniculata including anti-inflammatory, anti-diabetes, anti-viral, and immune stimulating pro-perties. The main objective is chromate-graphic evaluation using High-Performance Thin Layer Chromatography (HPTLC) to analyze the chemical composition of Andrographis paniculata. The HPTLC method is detailed, which is used in qualitative analysis of Andrographis paniculata. The article concludes with the qualitative analysis of Andrographis paniculata, comparing chromatograms in different solvents and wavelengths. Methanol is identified as the superior solvent providing a clearer chromatogram. Chemical constitution analysis reveals the number of visible chemicals at different wavelengths, offering insights into the herb's composition. The study provides valuable information for pharmaceutical quality control and the analysis of medicinal plant.

Facile, sensitive and reagent-saving smartphone-based digital image colorimetric assay of captopril tablets enabled by long-pathlength RGB acquisition

A new assay of captopril (CTP) tablets was developed based on digital image colorimetry using Ellman’s reagent. For the first time, a facile technique of increasing the analytical path was applied in this work to enhance the sensitivity. For this purpose, the reaction solutions were photographed using a smartphone while they were contained in two 1-cm pathlength cuvettes which were placed side by side. The Red-Green-Blue (RGB) in term of [B/(R+G+B)] was used to plot a standard curve. Compared to using a single cuvette, double cuvettes resulted in more precise analytical signals and better linearity (r2 of 0.9992). Additionally, CTP could be analyzed at low concentrations (2.5–25 µM) with LOD of 0.70 µM and LOQ of 2.13 µM, thus lowering the reagent consumption. The assay was proven to be valid, and it was greener, faster, and more affordable than the pharmacopeial chromatographic method, thereby suitable for pharmaceutical quality control.