Analytical Development Research Articles

Analytical Method Development and Dermal Absorption of 4-Amino-3-Nitrophenol (4A3NP), a Hair Dye Ingredient under the Oxidative or Non-Oxidative Condition

The chemical 4-amino-3-nitrophenol (4A3NP) is classified as an amino nitrophenol and is primarily utilized as an ingredient in hair dye colorants. In Korea and Europe, it is exclusively used in non-oxidative or oxidative hair dye formulations, with maximum allowable concentrations of 1% and 1.5%, respectively. Despite this widespread use, risk assessment of 4A3NP has not been completed due to the lack of proper dermal absorption data. Therefore, in this study, both the analytical method validation and in vitro dermal absorption study of 4A3NP were conducted following the guidelines provided by the Korea Ministry of Food and Drug Safety (MFDS). Before proceeding with the dermal absorption study, analytical methods were developed for the quantitation of 4A3NP through multiple reaction monitoring (MRM) via liquid chromatography-mass spectrometry (LC-MS) in various matrices, including swab wash (WASH), stratum corneum (SC), skin (SKIN, comprising the dermis and epidermis), and receptor fluid (RF). These developed methods demonstrated excellent linearity (R2 = 0.9962–0.9993), accuracy (93.5–111.73%), and precision (1.7–14.46%) in accordance with the validation guidelines.The dermal absorption of 4A3NP was determined using Franz diffusion cells with mini-pig skin as the barrier. Under both non-oxidative and oxidative (6% hydrogen peroxide (H2O2): water, 1:1) hair dye conditions, 1% and 1.5% concentrations of 4A3NP were applied to the skin at a rate of 10 μL/cm2, respectively. The total dermal absorption rates of 4A3NP under non-oxidative (1%) and oxidative (1.5%) conditions were determined to be 5.62 ± 2.19% (5.62 ± 2.19 μg/cm2) and 2.83 ± 1.48% (4.24 ± 2.21 μg/cm2), respectively.

Analytical method development and dermal absorption of gallic acid, a hair dye ingredient

Analytical method development and dermal absorption of gallic acid, a hair dye ingredient

The past is the future: from natural acid-base indicators to natural reagents in sustainable analytical chemistry

Abstract This article reviews the use of natural resources in analytical chemistry throughout history. Plant extracts were employed as indicators in chemistry for identifying the acidity or alkalinity of liquids as early as the 1650s. Later, as the industrial revolution altered people’s lives, synthetic chemicals were used instead. Modern techniques of analysis have replaced conventional ones as a result of advancements in physics and technology. The industrial revolution was an era of excitement until the toxic pollutants released from industries severely damaged people and the environment. The concepts of green chemistry and green analytical chemistry were proposed as potential solutions to the problems. The use of natural extracts as chemical analysis reagents has been reconsidered recently as a sustainable alternative. While new technologies such as artificial intelligence (AI) will influence future trends in analytical chemistry development, the primary goal is to move toward sustainable analytical chemistry, which includes using natural reagents and reducing the amount of chemicals consumed and waste produced.

Procjena utjecaja matriksa na kvantifikaciju lipofilnih toksina u plodovima mora

Phycotoxin accumulation in seafood can cause human intoxication and significant economic losses in seafood-producing areas. To protect consumer safety, maximum permitted levels in bivalve molluscs have been set, with appropriate analytical methods for their determination and quantification. The reference method for lipophilic phycotoxins, commonly referred to as lipophilic toxins, is liquid chromatography tandem mass spectrometry (LCMS/MS method), where coeluting components from the matrix can affect the efficiency of ionisation, resulting in erroneous quantification. In this study, the matrix effect was evaluated using the slope ratio analysis method, which involves comparing the slopes of the calibration curves in the matrix with those in pure solvent. The extent of the matrix effect was investigated in mussels, oysters, queen scallops and ascidians. The study covered all phycotoxins under Regulation EU 853/2004 for which certified standards are commercially available, including unregulated pectenotoxin 2. The results indicated that all lipophilic toxins were susceptible to this effect when LC-MS/MS was used for their determination. Significant ion suppression was evident for most analytes in all matrices, except for okadaic acid and dinophysistoxin 2 in bivalves, where significant ion enhancement was demonstrated, and dinophysistoxin 1 in oyster and scallop extract where no significant effect on ionisation was observed. Further analysis revealed no significant differences between the slope of mussel matrix-matched calibration and that of other bivalve matrices. Given this minor difference, the mussel matrix-matched calibration curve could be applied to minimise the matrix effect and to quantify phycotoxins in bivalve matrices analysed here, with the exception of the okadaic acid group in ascidians, which requires matrix-matched calibration prepared with the blank extract of these mentioned species. Given the risks phycotoxins pose to human health, ongoing analytical method development is necessary in this field to properly control food safety and ensure consumer health.

Approaches for sustainable professional skill development for vocational education students in Thailand

Background This article presents a research study that aims to explore sustainable approaches for developing professional skills in vocational education students in Thailand. This is the second phase of the research, which utilizes a qualitative research methodology. Methodology The key informants in this study are administrators of vocational education institutions, teachers, and students currently enrolled in vocational education institutions in Thailand, totaling 36 participants. The research uses a purposive sampling method and snowball sampling method. Data collection methods include document analysis, in-depth structured interviews, and observation. The results of the interviews are analyzed, and the content analysis is summarized. The research process consists of 4 steps: 1) literature review, 2) data collection, 3) data analysis, and 4) verification and confirmation. Results The research findings highlight several key considerations, including: 1) factors influencing the development of professional skills among vocational education students, such as curriculum design, support and counseling, practical training in workplaces, interactive learning, problem-solving and analytical thinking skills development, practical learning, and supportive learning environments, 2) approaches for sustainable professional skill development involve employing the appropriate approaches for self-development. The steps include setting clear goals and plans, active learning and training, technology skill development, experiential learning, problem-solving skill development, participation in professional activities, self-reflection, and continuous self-improvement. Conclusion These approaches aim to enhance the competencies of vocational education students, ensuring quality and efficiency as part of lifelong learning and sustainable development.

Stability indicating high performance thin layer chromatography method development and validation for quantitative determination of tetracycline hydrochloride in tetracycline hydrochloride active pharmaceutical ingredient (API) and its dosage forms

Simple, quick, cost-effective, and environmentally friendly analytical methods for quality assurance and control roles for different medicines, including Tetrcyclines, are most significantly needed. Also, different thin layer chromatography (TLC)-based methods for tetracycline identification exist, but high performance thin layer chromatography methods based on modern state- of- the art equipment are still nonexistent. Thus, in this study, analytical method development and verification were done by high performance thin layer chromatography (HPTLC) (using an automated equipment model) using glass plates coated with silica gel 60 F254 after treating with 10% Na2EDTA. Validation was carried out according to International Council for Harmonization (ICH) guidelines. A mobile phase formed from ethyl acetate, acetonitrile, methanol, and 1% aqueous ammonia in the composition of 4.4:19.6:10:6 volume to volume ratio (V/V) was used. Rf value, percentage recoveries, linearity ranges, limit of detection (LOD), and limit of quantitation (LOQ) for the developed HPTLC method were 0.28, 100.83–106.25%, 160–560 ng/band (r2 values of 0.9999), 31.9 ng/band, and 96.7 ng/band, respectively. The results of the sample assays conducted using the new method and the United States Pharmacopoeia (USP) high performance liquid chromatography (HPLC) method were 91.59% to 108.3% and 90.83% to 102.85%, respectively. The F test for the aforementioned methods was 2.01, which is smaller than the tabulated F value of 5.05 with 5 degrees of freedom at a 95% confidence range, proving that the newly developed HPTLC and HPLC pharmacopoeial methods can be used interchangeably.The newly developed HPTLC method is easy, economical, specific, accurate, and roboust, thus it can be employed in a range of settings that require quality control and assurance activities of tetracycline hydrochloride (TC-HCl) in bulk and ointment dosage forms.

Recent progresses in analytical method development for 210Pb in environmental and biological samples.

As a decay product of uranium series, 210Pb spreads widely in the nature and imposes strong radiological and chemical toxicity. It is vital to establish reliable and efficient radioanalytical methods for 210Pb determination to support environment and food radioactivity monitoring programs. This article critically reviews analytical methods developed for determining 210Pb in environmental and biological samples, especially new development in recent years. Techniques applied throughout different analytical steps including sample pretreatment, separation, purification, and detection are summarized and their pros and cons are discussed to provide a holistic overview for 210Pb environmental and biological assay.

Organophosphate esters and their metabolites in marine fish from Vietnam: Analytical method development and validation

Organophosphate esters (tri-OPEs), which are a significant group of emerging organic pollutants, have been widely found in aquatic products worldwide. While tri-OPEs have been extensively detected in aquatic products and are known to represent potential risks to human health, there is limited information available regarding their metabolites (di-OPEs). Currently, the techniques for analyzing the composition of tri- and di-OPEs have been distinguished and have certain drawbacks in terms of their expense, time requirements, and reliability. The objective of the study is to develop, validate, and utilize a modified QuEChERS technique for extracting tri- and di-OPEs in marine fish. As a result, EMR-Lipid and WAX were selected as adsorbents for the QuEChERS method to purify the samples and a combination of centrifugal vacuum and nitrogen at a temperature of 1 °C was selected as a technique to enhance the sensitivity of the developed method. The parameters of the method validation are in accordance with the criteria specified in SANTE/11312/2021 (a recovery ranging from 84.0% to 107.4% and RSD of precision below 20%). The aforementioned methodology was employed to assess the tri-OPEs and their metabolites in a total of 72 fish muscle samples obtained from the presence of OPEs in all recorded instances. The average concentration of ΣOPEs was determined to be 87.4±55.0 ng/g dw, with TBOEP and BEHP identified as the predominant compounds. Furthermore, no significant variation in the content of tri- and di-OPEs was observed in fish samples, regardless of species or geographical location.

Rapid, Simple and Low-Cost Analytical Method Development for Quantification of Eltrombopag Olamine in Tablet dosage by UV Spectroscopy Method

Rapid, Simple and Low-Cost Analytical Method Development for Quantification of Eltrombopag Olamine in Tablet dosage by UV Spectroscopy Method

Analytical Method Development and Validation of Brivaracetam in API and Marketed Formulation by RP-HPLC

A rapid and precise reverse phase high performance liquid chromatographic method has been developed for the validated of brivaracetam in its pure form as well as in tablet dosage form. Chromatography was carried out on a Symmetry ODS RP C18,5mm, 15mm x 4.6mm column using a mixture of phosphate buffer: methanol: acetonitrile (30:35:35% v/v) as the mobile phase at a flow rate of 1.0ml/min, the detection was carried out at 285 nm. The retention time of the brivaracetam was 2.183. The method produces linear responses in the concentration range of 60-140μg/ml of brivaracetam. The method precision for the determination of assay was below 2.0%RSD. The method was found to be sensitive, accurate and precise useful in the quality control of bulk and pharmaceutical formulations.  

FilmCrit: using cinematic critical race counterstorytelling as critical race feminista methodology

This paper provides an overview of a Critical Race Feminista praxis-oriented methodological framework in development called FilmCrit, and a critical race method expanded into filmic form called Cinematic Critical Race Counterstorytelling. Critical Race Feminisita Praxis informs this work by drawing on a Critical Race Theory in Education framework and Chicana Feminist theories and epistemologies. In discussing two FilmCrit studies, a qualitative documentary study, No Somos Famosos (We Are Not Famous), and my dissertation study, From the Classroom to the Screen: Experiences of Women of Color MFA Film Students, I detail the theoretical, methodological, and analytical development, as well as the scholarly significance, of FilmCrit and (auto)biographical and composite Cinematic Critical Race Counterstorytelling.

Therapeutic Potential, Pharmacological Activities and Analytical Aspects of Liriodendrin in Medicine: Novel and Potential Therapy Options for the Treatment of Human Disorders and Associated Complications

Abstract:: Natural products and their derived secondary metabolites play an important role in medicine and other allied health sectors. Liriodendrin is one of the main lignans of Boerhaavia diffusa roots. Liriodendrin is a lignin class phytochemical having numerous health beneficial properties in medicine, including anti-myocardial ischemia, anti-arrhythmic, anti-oxidant and anti- inflammatory potential. This present review aims to analyze the reported ethnomedicinal properties, pharmacological activities and analytical aspects of liriodendrin and identify the remaining gaps in medicinal fields for their future investigations. The pharmacological properties of liriodendrin have been described in the present paper in order to describe its better utilization in natural medicine in the future. Biological poptential and pharmacological activities of liriodendrin have been described in the present work with their analytical development in the scientific fields. In the present work, scientific data on liriodendrin were collected from different scientific databases such as PubMed, Springer, Google, Science Direct, and Google Scholar. They described their biological potential on the basis of the available scientific literature. Further, research and review articles from peer-reviewed journals were also searched during data collection. The present paper's scientific data signified the biological importance of liriodendrin in medicine, which has been isolated from Boerhaavia diffusa and other medicinal plants. Liriodendrin has biological potential against myocardial infarction, arrhythmias, lung injury, hepatic injury, antiinflammatory, ulcerative colitis, gastric injury, SARS-CoV-2 protease and intestinal inflammation. Further, its effectiveness in medicine was also due to its anti-convulsant activity, nitric oxide inhibitory potential, cytotoxicity, cytoprotective nature, anti-oxidant, and anti-microbial potential. The present paper's scientific data also described the metabolism and analytical development for their isolation, separation and identification in different samples. Detailed pharmacological activities of liriodendrin have been described here in the present work and highlighted its important pharmacological properties and analytical aspects. Liriodendrin is a valuable phytochemical of Boerhaavia diffusa, which has numerous biological applications in medicine. Further, this study can also validate the traditional and ethnobotanical use of the Boerhaavia diffusa and other plant material, which contain a significant amount of liriodendrin as an active phytochemical. Liriodendrin have huge biological potential far beyond its traditional uses in human complications.

Thermal Behavior of Solid Heated by Gaussian Moving Heat Source

In this paper, an analytical development is proposed to explicitly calculate the three-dimensional and transient temperature of a solid heated by a Gaussian moving heat source. The moving source dissipates heat in a thin layer near the irradiated surface of the solid and can be constant or pulsed or have any time evolution, depending on the application. The resulting solution requires only one convergent integral over time, which can be quickly computed numerically using, for example, a commercial formal calculation software. On the other hand, the derivative of the temperature with respect to time is fully explicit. We show that the results of the developed analytical solution are in excellent agreement with those of a numerical modeling that we performed under the same conditions. The temperature evolutions and the thermal maps are presented and commented.

Comparison of Protein-like Model Particles Fabricated by Micro 3D Printing to Established Standard Particles

Innovative analytical instruments and development of new methods has provided a better understanding of protein particle formation in biopharmaceuticals but have also challenged the ability to obtain reproducible and reliable measurements. The need for protein-like particle standards mimicking the irregular shape, translucent nature and near-to-neutral buoyancy of protein particles remained one of the hot topics in the field of particle detection and characterization in biopharmaceutical formulations. An innovative protein-like particle model has been developed using two photo polymerization (2PP) printing allowing to fabricate irregularly shaped particles with similar properties as protein particles at precise size of 50 µm and 150 µm, representative of subvisible particles and visible particles, respectively.A study was conducted to compare the morphological, physical, and optical properties of artificially generated protein particles, polystyrene spheres, ETFE, and SU-8 particle standards, along with newly developed protein-like model particles manufactured using 2PP printing.Our results suggest that 2PP printing can be used to produce protein-like particle standards that might facilitate harmonization and standardization of subvisible and visible protein particle characterization across laboratories and organizations.

Supporting resilient communities in the Pacific

Pacific Island communities are disproportionally impacted by the effects of climate change, and as teina (younger sibling) to our Pacific tuakana (older sibling), it is our responsibility to ensure these communities have resilience through co-developed solutions to these real-world problems. We focus on marine and freshwater ecosystems, understand their intrinsic links to Pacific communities, while, in partnership with science, empower and enable local knowledge to steer the waka. With more than 20 years’ experience of supporting Pacific communities, we deliver our positive impact through knowledge exchange, capability and capacity development, and problem solving. We strive to learn and grow our own capability, while brokering knowledge between Aotearoa, the Pacific, and our world leading research partners. Our aim is that Pacific Island communities gain a deeper scientific understanding of their aquatic systems, have the tools to rejuvenate and conserve these ecosystems, are empowered to transform their food systems towards more healthy, sustainable, and resilient pathways, and can adapt to the impacts of climate change. We take a systems approach that incorporates adaptive solutions, which are community-led, thereby ensuring a long-lasting positive impact into the future. Our Kete is filled with world-leading expertise from different organizations, which ensures a greater collective impact where it is needed most. This presentation will cover the seven themes within our Pacific Impact area, with a particular focus on food safety and security in relation to ciguatera poisoning (the number one cause of non-bacterial seafood illness affecting Pacific Island communities) (1,2), analytical laboratory development, and transforming food systems.

Analytical Method Development and Validation of a UV‐Spectrophotometric Technique for Pioglitazone HCL Estimation in Bulk and Polymeric Nanoparticles

AbstractThe type 2 diabetes drug pioglitazone is encapsulated in polymeric (Chitosan/PEG blended PLGA) nanoparticles utilizing solvent evaporation methods. The current research aimed to develop and validate an accessible, accurate, fast, and commercial UV spectrophotometric approach for assessing Pioglitazone in bulk and polymeric nanoparticles. In the estimation method that involves a pH 7.4 phosphate buffer, the maximum absorbance of Pioglitazone is reported to be 269 nm. With a correlation coefficient of 0.999, the drug exhibits linearity in the concentration series of 5–60 µg mL‐1. The proposed technique is validated as per ICH guidelines for linearity, accuracy, precision, and ruggedness. When the proposed technology is used in nano‐formulation, the percent amount of drug estimated to be 99.35% agreed well with the label claim. Recovery experiments at three distinct levels, 50%, 75%, and 100% are used to test the method's accuracy. The recovery rate is estimated to be between 98.91% and 99.11%. The low percent relative standard deviation (RSD) value indicates the method's accuracy and reproducibility. The method's repeatability, intraday, and interday precision are all examined. The approach is precise if the percent RSD value is less than 2. With the assistance of two analysts, the ruggedness of the suggested method is investigated. For the scheduled examination of Pioglitazone in bulk and polymeric nanoparticles, the above process has been developed and validated and proved to be a quick and cost‐effective quality‐control tool in pharmaceuticals.

The Quality by design Approach for Analytical Method Development and Validation of the RP-HPLC Method for Estimation of Quercetin in Pure, Marketed, and Cream Formulation

ABSTRACT: A simple, precise reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for the flavonoid quercetin, isolated from Tridax procumbens L. The method was validated by using Phenomenex C18 (250 x 4.6mm i.d) Column. A simple, cost effective mobile phase consisting of (ACN and 10 m/moL Phosphate buffer as mobile phase in proportion of 50:50 v/v ) pH 3, 1.0 ml/min Flow rate at 370nm by using UV Visible detector. The retention time of Quercetin was found to be 3.392 minutes. The Quercetin linearity range was found to be 05 to 25 μg/mL. The accuracy and precision of commercially available preparations and in-house cream formulations were investigated using a one-way ANNOVA test. The Percentage recovery of both formulations was found to be 99.83%, 99.88%, 99.82% and 98.92%, 98.18%, 98.86%. Robustness of analytical method was studied by using 2/3 full factorial design by using Design expert software. The Percentage assay and % RSD of marketed capsule and in house cream was found to be 98.38 %, 97.40% and 0.05273, 0.02053 respectively. The Limit of Quantitation and Limit of detection were found to be 0.9053μg/mL and 2.5435μg/mL respectively. The development method of quercetin is simple, accurate, precise, sensitive, and robust

Analytical Method Development and Validation Of Stability Indicating RP-HPLC Method For Assay and Related Substances of Paracetamol and Caffeine Effervescent Tablets: Review

he ongoing, interdependent tasks related to the departments of research and development, quality control, and quality assurance are the creation and validation of analytical methods. Analytical methods are essential for risk management and equivalency assessments. It aids in the development of acceptability standards unique to a product and the consistency of outcomes. Validations establish whether the analytical process is appropriate for the goal for which it was designed. A review of the literature indicates that paracetamol and caffeine can be determined individually or in combination with other medications using analytical techniques based on UV spectroscopy, RP-HPLC, and HPTLC. The parameters were checked for correctness, precision, robustness, and other aspects of analytical validation in accordance with ICH guidelines. The discovered techniques can be applied to the bulk and tablet dosage form analysis of paracetamol and caffeine in effervescent form since they are straight forward, sensitive, and repeatable. The review also outlines the applicability and constraints of numerous published analytical techniques for paracetamol and caffeine analysis. Stability studies have to be conducted on time and in compliance with the standards issued by the World Health Organization, International Conference of Harmonization, and other bodies. The capacity of a pharmaceutical product to meet the physical, chemical, microbiological, toxicological, protective, and informational requirements of a specific formulation in a particular container-closure system is known as its stability. It also ensures that a pharmaceutical product's effectiveness, safety, and performance will be maintained for the duration of its shelf life, which is seen as a need for approval and acceptability. The requirement for ongoing quality and purity monitoring of medications and products gave rise to various stability test techniques. This review covers the various drug substance stability categories as well as the applicability of various techniques for drug substances that are stable, the applicability of various methods used to test the pharmaceutical product's stability, guidelines released to test the pharmaceutical product's stability, protocols for stability testing that outline the essential elements of a well-managed and regulated stability test, and other aspects of stability are all covered in this review. The researcher working on paracetamol and caffeine in effervescent form will greatly benefit from this thorough review study.

Green Analytical HPLC Method Development of Acyclovir Loaded Floating Raft Formulation in Spiked Rabbit Plasma

Objective: The need of this investigation is to design eco-friendly, sensitive, and precise bioanalytical high-performance liquid chromatography (HPLC) techniques that leverage green analytical tools such as green analytical procedure index (GAPI), analytical eco scale (AES), and analytical greenness metric (AGREE) to analyze ACV-spiked rabbit plasma and ACV-loaded floating raft formulation (FRF) because The literature survey revealed insufficient data for the HPLC approach to FRF. Method: Methods involving plasma spikes mirroring the in-vivo models provide insights into potential real-life scenarios and the functionality of floating raft formulations loaded with ACV. The Design Expert tool optimized critical process parameters and identified significant factors influencing the chromatographic technique. Results: The CCD was used to optimize the flow rate (0.6 mL/min) and buffer solvent ratio (99:1) for separation. The C18 column (250 X 4.6 mm) was utilized to achieve the elution of ACV. The developed method was thoroughly validated through ICH guidelines. The ACV, lower limit of detection (LLoD), and lower limit of quantitation (LLoQ) retention times were established at 2.3 minutes, 15, and 20 ng/mL, respectively. Discussion: In summary, the study demonstrated the exceptional performance sensitivity, specificity, and robustness of the bioanalytical method. The method proved highly effective in quantifying ACV in plasma samples in terms of revalidatability, transferability, reproducibility, and the product development cycle. The developed method proves that using both design of experiments (DoE) and green analytical chemistry together creates a valid, eco-friendly, and reliable way to analyze the making of an ACV-loaded floating raft formulation.

Novel analytical method development and validation for simultaneous estimation of curcumin, ascorbic acid and salicylic acid in bulk and its pharmaceutical formulation by RP-HPLC

Novel analytical method development and validation for simultaneous estimation of curcumin, ascorbic acid and salicylic acid in bulk and its pharmaceutical formulation by RP-HPLC