Analytical Standards Research Articles

Introduction of curvature index and improvement of calibration curves used in ion chromatography (IC), atomic absorption spectrometry (AAS), UV-Vis spectrophotometry and catalytic combustion

The calibration curve represents the relationship between known CRM and the response of the instrument (e.g absorbance). Most of the time, in analytical chemistry standards, the linear function (of the 1st degree) is used to characterize the calibration curves. This, at first glance, has some major advantages: simple equation, simple linearity estimation criterion, and easy way of calculation. However, from a quality point of view, the grade 1 calibration curve does not characterize a working domain very well, because it does not take into account the curvature and has larger residuals. Here we show that, most of the time, the non-linear secondary function fits the calibration curves much better (argument valid for UV-Vis spectrophotometry, atomic absorption spectrometry (FAAS and ETAAS), catalytic combustion and ion chromatography (IC)), having lower residuals, but also a higher coefficient of determination, R2. The limitation of the secondary non-linear function use is given by the insufficiency of data related to its qualitative characterization. Through this work, we have introduced new characterization criteria for non-linear secondary functions such as curvature angle and curvature index. Although in the specialized literature, the term linearity of the calibration curve has existed for a long time, in reality it has not been fully interpreted. The curvature index developed in this work allows the controlled implementation of non-linear curves, but also with increasing the precision of the results. The curvature index characterizes the degree of curvature of the 1st or 2nd degree calibration functions. Using the 2nd degree calibration function allows the improvement of the obtained results, and curvature parameters (curvature angle and curvature index) allow qualitative characterization of many data sets used for calibration. The degree of curvature of a calibration curve is a new term not found in the literature, which will allow their characterization from a qualitative point of view.

Transformative knowledge of polar polycyclic aromatic hydrocarbons via high-resolution mass spectrometry.

Polycyclic aromatic hydrocarbons (PAHs) are toxic contaminants with a widespread presence in diverse environmental contexts. Transformation processes of PAHs via degradation and biotransformation have parallels in humans, animals, plants, fungi, and bacteria. Mapping the transformation products of PAHs is therefore crucial for assessing their toxicological impact and developing effective monitoring strategies. The present research aimed to explore the PAH detoxification products formed by the marine fish Atlantic haddock (Melanogrammus aeglefinus) after single PAH treatments. Using target and suspect screening analyses on an ion mobility quadrupole time-of-flight mass spectrometer (IM-QTOF MS), deprotonated compounds were identified and archived into a metabolite mass spectral library, which is systematized and presented in this work. The results offer an exclusive overview of the transformation products and their associated mass spectral features. Transformation products include hydroxy compounds, dihydrodiols, polycyclic aromatic acids, glucuronides, sulfates, glutathiones, cysteinylglycines, cysteines, and mercapturic acids. By documenting high-resolution mass spectrometry data, this comprehensive characterization provides a valuable reference point for the development of broad-spectrum analytical methods. It also addresses a critical gap in the field by presenting tentative identifications of PAH transformation products in the absence of analytical standards. Moreover, it encourages further investigation of these compounds as they have important toxicological relevance in both ecotoxicology and human research.

Pollen Analysis of Elaeis guineensis-Dominated Honeys in Lower Casamance: Floral Diversity and Honey Typology

Background: A honey's pollen spectrum serves as an indicator for determining its place of origin in terms of vegetation resources. This data might be utilised to create pollen analytical standards, which would help certify honey. The melliferous plants are plant species on which the bee takes substances, including nectar, pollen and resin to feed and to develop its various products (honey, royal jelly...). Aim: The aim of this study was carried out to contribute to melliferous plants in Casamance (Senegal) : pollen spectrum of honeys with Elaeis guineensis dominant. Results: Pollen analysis of 14 samples of dominant Elaeis guineensis honey from Lower Casamance in the Ziguinchor region identified 25 plant taxa in 11 families foraging for bees. The species richness varied from 5 to 10 taxa per honey sample. The most representative families are Fabaceae with 7 species, followed by Malvaceae with 3 species, Combretaceae, Myrtaceae, Rubiaceae, Poaceae, Arecaceae, Lamiaceae with 2 species and Avicenniaceae, Méliaceae, Asteraceae with 1 species. Pterocarpus erinaceus is present in 11 spectra including 7 spectra where it is isolated and in 3 spectra where it is isolated. It is the only taxon that is a companion pollen in 1 of the spectra. The most common taxa associated with Elaeis are Detarium senegalense, Daniellia oliveri and Myrtaceae. Conclusion: The data reflects the floral situation of the place were particular honey was produced and the identification of geographical origin based on the presence of a combination of pollen types of that particular area.

Protein “purity,” proteoforms, and the albuminome: critical observations on proteome and systems complexity

IntroductionThe identification of effective, selective biomarkers and therapeutics is dependent on truly deep, comprehensive analysis of proteomes at the proteoform level.MethodsBovine serum albumin (BSA) isolated by two different protocols, cold ethanol fractionation and heat shock fractionation, was resolved and identified using Integrative Top-down Proteomics, the tight coupling of two-dimensional gel electrophoresis (2DE) with liquid chromatography and tandem mass spectrometry (LC-MS/MS).Results and discussionNumerous proteoforms were identified in both “purified” samples, across a broad range of isoelectric points and molecular weights. The data highlight several concerns regarding proteome analyses using currently popular analytical approaches and what it means to (i) purify a “protein” if the isolate consists of a wide variety of proteoforms and/or co-purifying species; and (ii) use these preparations as analytical standards or therapeutics. Failure to widely recognize and accept proteome complexity has likely delayed the identification of effective biomarkers and new, more selective drug targets. iTDP is the most logical available analytical technique to effectively provide the necessary critical depth and breadth for complex proteome analyses. Routine analyses at the level of proteoforms will provide the much-needed data for the development and validation of selective biomarkers and drugs, including biologics.

ІНТЕГРОВАНЕ ПРОЄКТУВАННЯ ХВОСТОВОЇ ЧАСТИНИ ФЮЗЕЛЯЖУ ЛІТАКІВ ТРАНСПОРТНОЇ КАТЕГОРІЇ

For the first time, when designing transport category aircraft with a tail cargo hatch, a method of integrated design and construction of the fuselage tail section has been developed and presented, which, using mathematically described parameters, allows the creation of a particular master geometry of the fuselage tail section for a specifically selected cargo door scheme. The method has been improved to allow the design of transport aircraft not only at the stage of creating a fundamentally new aircraft concept, but also as a means of modifying an existing passenger aircraft type through deep modernization. A systematization and classification of existing types of cargo doors of the transport category aircrafts according to their design features has been developed. A separate group of tail cargo doors has been identified. Five typical schemes of cargo hatches in the tail section of the fuselage have been formed. A universal parametric method for specifying the master geometry of the fuselage tail section has been created, which allows the implementation of any of the above schemes of cargo doors in the fuselage tail section, including a unique one, implemented only on AN aircraft with a rolling ramp. The relationship between the parameters of the cargo door and the transportation characteristics of the aircraft, which depend on the range and types of cargo to be transported, methods of loading and unloading, and airdropung, is described. The methods of three-dimensional parametric modeling of both the tail sections of the fuselage and transport aircraft as a whole were further developed when creating a master geometry, a space distribution model, analytical standards of airframe structural elements, and a model for the complete determination of the geometric parameters of the aircraft using CAD/CAM/CAE/PLM technologies. The presented results have been implemented in the practice of designing transport category aircraft at ANTONOV Company, as well as at the National Aerospace University named after M.E. Zhukovsky “Kharkiv Aviation Institute” in the educational process of training aviation specialists.

The State of the Art in Post-Mortem Redistribution and Stability of New Psychoactive Substances in Fatal Cases: A Review of the Literature

In post-mortem (PM) investigations, forensic toxicologists attempt to identify legal or illegal substances present before death and determine how they contributed to the cause of death. A critical challenge is ensuring that PM sample concentrations accurately reflect those at the time of death, as postmortem redistribution (PMR) can alter these levels due to anatomical and physiological changes. The PMR phenomenon is called a ‘toxicological nightmare’. PMR significantly affects post-mortem drug concentrations, particularly for lipophilic drugs and those with a high volume of distribution. The emergence of new psychoactive substances (NPSs) has led to a growing recognition of their role as a significant public health concern, frequently associated with fatalities related to polydrug use. These substances are renowned for their ability to induce intoxication at low doses, which has led to the continuous updating of toxicological and forensic methods to improve detection and adopt new analytical standards. The comprehensive detection of NPS metabolites, some of which are still undiscovered, presents an additional analytical challenge, as do their metabolic pathways. This complicates their identification in fatal cases using standard analytical methods, potentially leading to an underestimation of their actual prevalence in toxicological results. Furthermore, the interpretation of analytical results is hindered by the absence of data on PM blood levels and the specific contributions of NPS to causes of death, exacerbated by the lack of knowledge of whether the PMR phenomenon influences them. This paper presents a comprehensive review of the literature on post-mortem cases involving various NPS, categorized according to classifications by the United Nations Office on Drugs and Crime (UNODC) and the European Union Drugs Agency (EUDA). These categories include cathinones, phenylethylamines, arylalkylamines, phencyclidine-type substances, phenmetrazines, piperazines, phenidates, aminoindanes, LSD-like NPSs, tryptamines, fentanyl analogs, designer benzodiazepines, synthetic cannabinoids, and nitazenes. This review covers not only postmortem blood levels but also the stability of the substances studied, the methods of analysis, and attempts to shed some light on the PMR phenomenon. This review used various key terms, such as PMR, NPS, and the names of previously categorized substances and drug analyses across multiple peer-reviewed journals and databases, including Scopus, Google Schoolar, Springer, PubMed, and Wiley Online Library. In addition, references from retrieved articles were examined to identify additional relevant research. Interpreting post-mortem toxicological results is complex and lacks definitive guidelines, requiring a nuanced understanding of its challenges and potential pitfalls. As a result, post-mortem toxicology is often regarded as an art. The primary aim of this review is to provide forensic toxicologists with a comprehensive framework to assist in the evaluation and interpretation of NPS analysis. This guide is intended to complement the existing knowledge and practices applied in forensic laboratories within the toxicological analysis of post-mortem cases.

ANALYTICAL PROFILING OF KUPIPAKVA RASAYANA – A REVIEW

Introduction: Though the Ayurvedic formulations are time tested for their promising and reliable therapeutic efficacy, there is a need for standardisation of the same in the current era to meet the global standards followed by global acceptance. A formulation must pass all the analytical tests before it enters the market, regardless of the system of medicine and dosage form, for the safe use of the drug. Analytical profiling in Kupipakva Ra-sayana (herbo-mineral preparations cooked in glass flasks under controlled heat) is essential for ensuring the safety, efficacy, and quality of these potent formulations used in Ayurveda, particularly Rasashastra. The com-plex processes and materials involved in Kupipakva Rasayana require a robust analytical assessment to validate their therapeutic use. Aim and Objectives: The study's main aim is to emphasise the importance of Analytical profiling in Kupipakva Rasayana. Materials and Methods: Concept of Kupipakva Rasayana, Instrumentation and SOP of each Analytical test for Kupipakva Rasayana, Impact of Analytical profiling in safety aspects, Need of Analytical profiling for Kupipakva Rasayana. Discussion: Though designing a formulation is the prime step in developing pharmaceutics, the analytical standardisation of the designed formulation encourages further prod-uct movement. Conclusion: Analytical profiling of Kupipakva Rasayana is essential because it decides the Pharmacodynamics and pharmacokinetics of the Drug thereby playing a significant role in therapeutic applica-tions

Analyzing the Effect of Resveratrol on Pharmacokinetics of Antituberculosis Drug Bedaquiline in Rats by a Novel UPLC-MS/MS Approach.

Bedaquiline (BDQ), a diarylquinoline compound, is an inhibitor of mycobacterial ATP synthase, specifically with FDA approval as a treatment for multidrug-resistant tuberculosis (MDR-TB). M2 is the main metabolite of BDQ and is active against tuberculosis. The objective of this study was to establish and validate a sensitive and convenient ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) approach to concurrently quantify BDQ and M2 in rat plasma and to examine whether resveratrol, a CYP3A4 inhibitor, could influence the pharmacokinetics of BDQ and M2 in rats. Plasma samples containing the internal standard (IS) linezolid were formulated by adding acetonitrile for a simple one-step protein precipitation, and the analytes in samples were quantified by the UPLC-MS/MS method. BDQ and M2 were successfully calibrated in the ranges of 0.5-1000 and 1.0-200 ng/mL, where the lower limit of quantification (LLOQ) was 0.5 and 1.0 ng/mL, respectively. The precisions and accuracies of BDQ and M2 were in compliance with the FDA analytical standards. Recoveries and matrix effects of the analytes were satisfactory, and the analytes remained stable under four different temperatures and conditions. The well-validated UPLC-MS/MS method was successfully applied to the study of the food-drug interaction in rats. Remarkably, resveratrol increased the level of exposure of BDQ. Furthermore, the effect of resveratrol on the metabolism of BDQ and M2 needs further clinical studies.

Detection of Regulated Ergot Alkaloids in Food Matrices by Liquid Chromatography-Trapped Ion Mobility Spectrometry-Time-of-Flight Mass Spectrometry.

Ion mobility mass spectrometry (IMS) acts as an additional separation dimension when integrated into liquid chromatography-mass spectrometry (LC-MS) workflows. LC-IMS-MS methods provide higher peak resolution, enhanced separation of isobaric and isomeric compounds, and improved signal-to-noise ratio (S/N) compared to traditional LC-MS methods. IMS provides another molecular characteristic for the identification of analytes, namely the collision cross section (CCS) parameter, reducing false positive results. Therefore, LC-IMS-MS methods address important analytical challenges in the field of food safety (i.e., detection of compounds at trace levels in complex food matrices and unambiguous identification of isobaric and isomeric molecules). Ergot alkaloids (EAs) are a family of mycotoxins produced by fungi that attack a wide variety of grass species, including small grains such as rye, triticale, wheat, barley, millet, and oats. Maximum levels (MLs) of these mycotoxins have been established in several foodstuffs, as detailed in the Commission Regulation EC/2023/915. This new legislation includes six main EAs and their corresponding epimers, so an efficient methodology is required to properly distinguish these isomeric molecules considering their co-occurrence. Therefore, the goal of this protocol is to show how the integration of IMS in LC-MS workflows contributes to the separation of isomeric EAs, enhancing the selectivity of the analytical method. Additionally, it illustrates how the generation of CCS libraries through the characterization of analytical standards provides higher confidence for the identification of mycotoxins. This protocol is designed to clearly explain the benefits of implementing IMS in food safety, taking as an example the determination of EAs in cereals. A QuEChERS-based extraction followed by an LC-trapped ion mobility spectrometry (TIMS)-MS analysis provided limits of quantification ranging from 0.65 to 2.6 ng/g with acceptable accuracy (although low recovery for ergotaminine) at 1.5x, 1x, and 0.5x the ML and exhibited a negligible matrix effect.

Latest trends in the environmental analysis of PFAS including nontarget analysis and EOF-, AOF-, and TOP-based methodologies.

Ubiquitous environmental occurrence of per- and polyfluoroalkyl substances (PFAS) underscores the critical need to broaden investigative efforts in effective screening, risk assessment, and remediation. Owing to thebroad spectrum of PFAS, various analytical techniques have been extensively utilized to attain inclusivity, with notable attention given to methods such as extractable organic fluorine (EOF), adsorbable organic fluorine (AOF), and the total oxidizable precursor (TOP) assay. These techniques expand the scope of PFAS analysis by estimating perfluoroalkyl acid precursors or the total organochlorine fraction. This review offers a comprehensive comparative overview of up-to-date methodologies, alongside acknowledging the inherent limitations associated with their applications. When coupled with target analysis via low-resolution tandem mass spectrometry, these techniques offer a potential estimation of total PFAS concentrations. Yet, analytical challenges such as the limited availability of reference analytical standards, partial PFAS adsorption, and the entrapment of fluorinated inorganic anions on adsorbent materials often restrict the comprehensiveness of PFAS analysis. So, integrating nontarget analysis using high-resolution mass spectrometry (HRMS) tools fortifies these PFAS mass balance approaches, enabling the development of a more holistic approach for anenvironmental analysis framework. This review provides additional insights into the comparative advantages of PFAS analytical approaches and explores various data prioritization strategies in nontarget screening methods. It advocates for the necessary optimization of PFAS extraction methods, asserting that integrating the nontarget approach would foster the establishment of a comprehensive monitoring framework across diverse environmental matrices. Such integration holds promise for enhancing scientific comprehension of PFAS contamination across diverse environmental matrices.

Deciphering Isotopic Fine Structures of Silylated Compounds in Gas Chromatography-Vacuum Photoionization Orbitrap Mass Spectrometry of Bio-Oils.

We introduce vacuum resonance-enhanced multiphoton ionization (REMPI) with high-resolution Orbitrap Fourier transform mass spectrometry (FTMS) for analyzing silylated polar compounds. UV laser radiation at 248 nm sensitively and selectively targets aromatic constituents, while high-resolution mass spectrometry (HRMS) enables high-performance mass spectrometric detection. This workflow enhances the detection confidence of polar constituents by identifying unique isotopologue patterns, including at the isotopic fine structure (IFS) level, in analytical standards and complex bio-oils. A direct and derivatized gas chromatography (GC) procedure on a polar standard component mixture allowed us to explore the general ionization and detection characteristics of REMPI FTMS. HRMS enabled the examination of the complex isotopologue profiles, revealing distinct patterns for the CHOxSiy-class compounds. Particularly in complex mixtures, this isobaric/isonucleonic complexity exceeded the classical mass resolution capabilities of the employed Orbitrap D30 series and prompted the usage of prolonged transients via an external data acquisition system. This procedure substantially improved mass spectrometric results by recording the unreduced time-domain transient data for up to 2 s. Notably, the ability to distinguish diagnostic isotopic pairs, such as 12C/29Si vs 13C/28Si with a mass split of ∼3.79 mDa and 13C12C/28Si29Si vs 13C2/28Si2, with an approximate mass difference of ∼3.32 mDa, demonstrates a significant and expected performance improvement. Finally, we benchmark the GC HRMS methodology to identify silylated oxygenated and nitrogen-containing constituents in ultracomplex bio-oil samples. The presented approach of utilizing the silicon isotope pattern and unique isotopologue mass splits for increasing attribution confidence can be applied beyond bio-oils toward the general GC analyses of polar oxygenates.

The Genus Commiphora: An Overview of Its Traditional Uses, Phytochemistry, Pharmacology, and Quality Control.

Myrrh is the resinous substance secreted by plants of the genus Commiphora. In traditional Chinese medicine, Ayurvedic medicine, and traditional Arabic medicine, myrrh is regarded as an important medicinal material, widely used in the treatment of trauma, arthritis, hyperlipidemia, and other diseases. This review explores the evolving scientific understanding of the genus Commiphora, covering facets of ethnopharmacology, phytochemistry, pharmacology, artificial cultivation, and quality control. In particular, the chemical constituents and pharmacological research are reviewed. More than 300 types of secondary metabolites have been identified through phytochemical studies of this genus. Guggulsterone is a bioactive steroid isolated mainly from Commiphora mukul. The two isomers, Z- and E-guggulsterone, have shown a wide range of in vitro and in vivo pharmacological effects, including anti-proliferation, antioxidant, anti-inflammatory, and antibacterial. However, the current scientific research on quality control of medicinal materials and identification of original plants is insufficient, which limits the reproducibility and accuracy of biological activity evaluation experiments. Therefore, the establishment of analytical protocols and standardization of extracts is an important step before biological evaluation. At the same time, in order to find more bioactive substances, it is necessary to strengthen the research on the stems, barks, and leaves of this genus. The sources used in this study include PubMed, CNKI, Web of Science, Google Scholar, and other databases, as well as multinational pharmacopoeias, ancient books of traditional medicine, herbal classics, and modern monographs.

A sustainable RP-HPLC method for simultaneously estimating aceclofenac, paracetamol, and serratiopeptidase with AQbD optimization

This study focused on developing and validating a novel method for the simultaneous estimation of aceclofenac (AFC), paracetamol (PCM), and serratiopeptidase (SPD) using reverse phase high-performance liquid chromatography (RP-HPLC). The method was designed based on Analytical Quality by Design principles, incorporating green and white analytical chemistry (WAC) to ensure environmental sustainability and analytical efficiency. The HPLC analysis was performed using an Agilent 1220 Infinity II system equipped with a PDA detector, binary solvent pump, and automatic injector. Separation was achieved on an Agilent Inertsil ODS 3 column (250 mm × 4.6 mm, 5 μm particle size) with a mobile phase of ethanol and a 10 mM phosphate buffer (pH 3), adjusted with 1 % orthophosphoric acid. A gradient elution method was employed with a flow rate of 0.8 mL/min and detection at 230 nm. The retention times for AFC, PCM, and SPD were found to be 3.5, 5.2, and 8.9 min, respectively. Method validation confirmed accuracy and precision, with relative standard deviation (RSD) values consistently below 2 %, and a linearity range that met acceptable analytical standards. The integration of green and white analytical chemistry principles enhanced the method's sustainability, reducing environmental impact while ensuring minimal revalidation requirements. By adopting WAC, the method demonstrated simplicity, stability, and a strong alignment with sustainable chemistry practices. This method serves as an innovative and environmentally friendly approach for the accurate analysis of pharmaceutical compounds.

Evaluation of the ionization efficiency in phosphatidylcholine positional isomers with docosahexaenoic acid bound to the sn-1 or sn-2 position

Phosphatidylcholine (PC), a key phospholipid, contains 2 fatty acids that can be bound at the sn-1 and sn-2 positions, resulting in positional isomers when different fatty acids are attached. Currently, there is no established method for identifying phospholipid molecular species and quantifying individual isomers using authentic standards of each PC isomer. In this study, we prepare authentic analytical standards for PC positional isomers through chemical synthesis and preparative purification. These isomers contain docosahexaenoic acid (DHA, 22:6) and palmitic acid (16:0) attached at the sn-1 and sn-2 positions and are denoted as PC(22:6/16:0) and PC(16:0/22:6), respectively. Standard solutions of PC(22:6/16:0) and PC(16:0/22:6) were analyzed using liquid chromatography-tandem mass spectrometry, and calibration curves of the PC positional isomers were generated to compare their ionization efficiencies. The ionization efficiency of PC(22:6/16:0) was 2.32 times higher than that of PC(16:0/22:6), indicating that the ionization efficiency depends on the binding position of the fatty acid. Elucidating and correcting the differences in the ionization efficiencies of the PC positional isomers will enable the accurate quantitative analysis of lipidomes in the future.

Providing quality-assessed and standardised soil data to support global mapping and modelling (WoSIS snapshot 2023)

Abstract. Snapshots derived from the World Soil Information Service (WoSIS) are served freely to the international community. These static datasets provide quality-assessed and standardised soil profile data that can be used to support digital soil mapping and environmental applications at broad scale levels. Since the release of the preceding snapshot in 2019, refactored ETL (extract, transform and load) procedures for screening, ingesting and standardising disparate source data have been developed. In conjunction with this, the WoSIS data model was overhauled, making it compatible with the ISO 28258 and Observations and Measurements (O&M) domain models. Additional procedures for querying, serving and downloading the publicly available standardised data have been implemented using open software (e.g. GraphQL API). Following up on a short discussion of these methodological developments we discuss the structure and content of the “WoSIS 2023 snapshot”. A range of new soil datasets was shared with us, registered in the ISRIC World Data Centre for Soils (WDC-Soils) data repository and subsequently processed in accordance with the licences specified by the data providers. An important effort has been the processing of forest soil data collated in the framework of the EU-HoliSoils project. We paid special attention to the standardisation of soil property definitions, description of the soil analytical procedures and standardisation of the units of measurement. The 2023 snapshot considers soil chemical properties (total carbon, organic carbon, inorganic carbon (total carbonate equivalent), total nitrogen, phosphorus (extractable P, total P and P retention), soil pH, cation exchange capacity and electrical conductivity) and physical properties (soil texture (sand, silt and clay), bulk density, coarse fragments and water retention), grouped according to analytical procedures that are operationally comparable. Method options are defined for each analytical procedure (e.g. pH measured in water, KCl or CaCl2 solution, molarity of the solution, and soil / solution ratio). For each profile we also provide the original soil classification (i.e. FAO, WRB and USDA system with their version) and pedological horizon designations as far as these have been specified in the source databases. Three measures for “fitness for intended use” are provided to facilitate informed data use: (a) positional uncertainty of the profile's site location, (b) possible uncertainty associated with the operationally defined analytical procedures and (c) date of sampling. The most recent (i.e. dynamic) dataset, called wosis_latest, is freely accessible via various web services. To permit consistent referencing and citation, we also provide a static snapshot (in this case, December 2023). This snapshot comprises quality-assessed and standardised data for 228 000 geo-referenced profiles. The data come from 174 countries and represent more than 900 000 soil layers (or horizons) and over 6 million records. The number of measurements for each soil property varies (greatly) between profiles and with depth, this generally depending on the objectives of the initial soil sampling programmes. In the coming years, we aim to gradually fill gaps in the geographic distribution of the profiles, as well as in the soil observations themselves, this subject to the sharing of a wider selection of “public” soil data by prospective data contributors; possible solutions for this are discussed. The WoSIS 2023 snapshot is archived and freely available at https://doi.org/10.17027/isric-wdcsoils-20231130 (Calisto et al., 2023).

Considerations for Measurements of Aggregate PFAS Exposure in Precision Environmental Health.

Per- and polyfluoroalkyl substances (PFAS) have become a major focus of research due to their widespread environmental presence and adverse health effects associated with human exposure. PFAS include legacy and emerging structures and are characterized by a range of functional groups and carbon-fluorine chains that vary in length (from fewer than 3 carbons to more than 7 carbons). Research has linked PFAS exposure to an array of health concerns, ranging from developmental and reproductive disorders to immune system impairments and an increased risk of certain cancers. In this new era of personalized health, measuring markers of PFAS exposure in human biospecimens is an important part of environmental public health surveillance. PFAS are typically measured in human blood and tissues using targeted approaches, which quantify individual PFAS structures using specific instrumentation. The diversity and complexity of PFAS, the limitations of the targeted approaches due to the sheer number of structures, and the absence of publicly available analytical standards pose significant challenges for measurement methodologies. This perspective aims to describe aggregate PFAS exposure measurements and their potential for use in precision medicine applications including a discussion of the limitations and potential benefits of these aggregate measurements. As public health organizations, healthcare professionals, and the public look for guidance regarding the safe use of and exposure to PFAS, in a pragmatic cost-effective manner, the dynamic field of measurement science is poised to respond with innovative technological solutions to an important public health need.

ANALYSIS AND STANDARDIZATION OF RASANJANADI TAILA: A STEP TOWARDS QUALITY CONTROL AND GLOBAL ACCEPTANCE

Analysis of Ayurveda formulations is crucial to identify the bioactive compounds, their concentrations, and in-teractions which affect their therapeutic efficacy and safety. Standardisation of these formulations is essential to ensure consistency in their composition, manufacturing pro-cess, and quality control, thereby guaranteeing their safety and efficacy. The quality and effectiveness of Ayurveda formulations can vary significantly due to the lack of standardised manufacturing processes and ana-lytical methods. Inadequate analysis and standardisation of Ayurveda formulations can result in adverse effects, interactions, and contamination, posing a risk to patient safety. Furthermore, the absence of standardisation can impede the development of new Ayurveda formulations and restrict their global acceptance. Rasanjanadi Taila, a traditional Ayurveda formulation, is specifically cited by Acharya Vangasena in the Nasarogadhikara chapter for the treatment of Pratishyaya (Rhinitis), which comprises Rasanjana, ShodithaAtivisha, Musta, and Devadaru. The formulation was prepared in accordance with the AFI standards for Taila preparation. These drugs are very potent individually, and the Taila contains many Teekshna Dravya in it. There are no analytical standards avail-able for Rasanjanadi Taila in AFI to check its quality. In this study, an effort has been made to prepare Rasanja-nadi Taila and analyze its physicochemical properties, phytochemical constituents, and microbial load to ensure its quality and efficacy.

Application of pattern deconvolution strategies for the estimation of bromochloro alkane concentrations in indoor dust samples

Bromochloro alkanes (BCAs) are a class of flame retardants similar in structure to polychlorinated alkanes (PCAs), which are the major component of short-chain chlorinated paraffins (SCCPs) listed as Persistent Organic Pollutants under the Stockholm Convention. BCAs have recently been detected for the first time in environmental samples. Due to the complete lack of commercially available analytical standards, no method for quantifying BCAs has been reported to date. In this study, 16 custom-synthesised standards with mixed bromine and chlorine halogenation and carbon chain lengths ranging from C10 to C17 were characterized by liquid chromatography and Orbitrap high-resolution mass spectrometry and used to assess the applicability of pattern deconvolution quantification strategies for BCAs in indoor dust. Br1-9 and Cl1-8 BCAs were detected as [M + Cl]– adduct ions among the C10 to C17 standards, as well as numerous PCA homologues. After applying correction factors to account for the presence of PCAs in the standards, triplicate fortification experiments using varied halogenation composition and concentration determined an average measurement accuracy of 81% over the carbon chain lengths studied and coefficient of variance ≤20% between replicates. Overall, approximately 89% of the ΣBCA concentrations quantified in the fortification trials met the European Union Reference Laboratory's accuracy acceptability criteria recommended for PCAs, between 50 and 150%. Application of the BCA pattern deconvolution quantification procedure to seven representative indoor dust samples from the United States of America revealed a low correlation between the homologue distribution in the samples and the prototype standards (R2 ≤ 0.40), which precluded reliable quantification. This study indicates that pattern deconvolution is an appropriate strategy for quantifying BCAs in environmental samples, but that a large set of appropriate mixture standards will be required before more reliable estimates of BCA concentrations can be achieved in indoor dust.

An interactive R-based custom quantification program for semi-quantitative analysis of triacylglycerols in bovine milk.

The R programming language, RStudio, and open-source software solutions for analysis of liquid chromatography-mass spectrometry (LC-MS) data have been used with user-written R-based custom quantification programs (CQP) for semi-quantification of triacylglycerols (TAGs) in bovine milk lipid extracts. Using the peak-finding capabilities of the package "xcms" in RStudio, peaks were integrated, and retention times aligned, normalized, and then used for semi-quantitative analysis of a custom set of four extraction internal standards (EISs) and 29 TAG regioisomers using the choice of four analytical internal standards (AISs). Alternating stereospecific numbering (sn) 1,3 TAG regioisomers (standards 1, 3, and 5 of six calibration standards) and sn-1,2 TAG regioisomers (standards 2, 4, and 6 of six standards) were used to make a set of six calibration standards, which were used for quantification using a linear fit model, polynomial fit model, power fit model, level-bracketed linear fit, replicate-bracketed polynomial fit, replicate-bracketed power fit, and replicate- and level-bracketed linear fit and response factors. For example, the linear fit for EIS1 gave an unacceptable coefficient of determination (CoD), r2 = 0.9616, whereas the polynomial fit gave r2 = 0.9908 and the power fit gave r2 = 0.9928, while the double-bracketed linear fit gave CoDs of r2 = 0.9960, 0.9848, and 0.9781 for the three brackets, yet gave the least % difference to known calibration concentrations. For unparalleled transparency, the CQP produced webpages that allowed every step in the data processing and quantification sequence to be verified and reproduced, and contained interactive figures. The data are publicly available using a digital object identifier (DOI). The R code can be downloaded and used with the downloadable data to reproduce the results, to modify the code and further customize the results, or to copy and paste and adapt the code to other quantification applications.

Production and Enrichment of Erucic Acid Methyl Ester Analytical Standards from Natural Oils for Food Control Analysis

Production and Enrichment of Erucic Acid Methyl Ester Analytical Standards from Natural Oils for Food Control Analysis