Sugars or saccharides exist as structural and stereo- isomers and can be difficult to analyse, due to insufficient analyte separation. By coupling chromatography with mass spectrometry, the reliability of the analysis can be improved, but there is still potential for erroneous results due to the vast array of saccharide isomers present in nature. In this study, we present a method for the analysis of 80 saccharides analysed using an ion chromatograph coupled to a mass spectrometer. The method successfully separated, identified and quantitated 21 monosaccharides, 28 disaccharides, 15 trisaccharides, 7 tetrasaccharides, and 9 sugar alcohols. The feasibility of this method was demonstrated through the analysis of commercially available rare and common sugar samples, as well as honeys. While the method showed promising results for these compounds, further validation will be required to determine its applicability in more stringent fields such as forensics and clinical analysis.

Methamphetamine is the most trafficked synthetic drug, with a significant proportion of its production originating from the precursor ephedrine/pseudoephedrine. Ephedrine/pseudoephedrine have their own production pathways, with novel synthetic routes appearing in reports. An investigation into chiral and stable isotope profiling of a novel synthesis to ephedrine via a carbamate protection-methylation pathway involving a lithium aluminium hydride reduction of carbamate protected phenylpropanolamine was performed. The combination of S13C and S2H values may allow for discrimination from other reported ephedrine-based routes. Likewise, the combination of S13C and S2H values may allow for discrimination from another recently reported novel ephedrine/pseudoephedrine carbamate protectionmethylation pathway. The S13C values were not as negative compared to the previously reported carbamate protection-methylation pathway. An investigation into the fractionation of 13C found a smaller negative shift during the methylation step which may reflect the source of the carbon group that carries out the methylation. Diastereomeric analysis confirmed ephedrine is formed and no presence of pseudoephedrine. Chiral analysis confirmed reduction of the ephedrine formed racemic methamphetamine.

Hexamine is a precursor chemical for commercial explosives such as RDX and HMX and homemade explosive such as HMTD and R-Salt. Although now controlled in some jurisdictions, hexamine was still available in Australia in the form of solid fuel tablets. The other ingredient of R-Salt, sodium nitrite, was available with few restrictions. We report the isotopic compositions of hexamine derived from solid fuel tablets and sodium nitrite available in 2024. The isotopic compositions for 18 samples of hexamine spanned wider ranges than previously reported: S2H from -179 to +104 %o, S13C from -49.7 to -25.0 %o and S15N from -6.5 to +3.7 %o. The nitrogen isotopic compositions of 17 samples of sodium nitrite ranged from -166.9 to +3.1 %o representing some of the most 15N depleted values reported for natural materials. 32 batches of R-Salt were synthesised from selected samples of hexamine and sodium nitrite. Progressing from hexamine to R-Salt, S2H values became more positive by between +5.2 and + 18 %o and S13C values became more positive by between +12.3 and + 14.6 %o. A combination of these data presents a means to associate samples of R-Salt with precursor hexamine. The contributions of hexamine and sodium nitrite to the nitrogen isotopic compositions of R-Salt were combined by a simple mass-balance equation. Using this model the S15N values of R-Salt were more negative than the combined precursors by between -2.0 and - 1.1 %o. This presents an additional means to associate samples of RSalt with both precursor chemicals.

This paper provides a decadal review of literature describing the analysis of simple saccharides and oligosaccharides in food by ion chromatography pulsed amperometric detection (IC/PAD) and ion chromatography mass spectrometry (IC/MS) as emerging techniques. The concentrations of these saccharides in food have important health implications and affect technical attributes of food quality. Saccharides have been analyzed over many decades using a diverse range of physical, chemical, and chromatographic techniques, each with their own advantages and disadvantages. In the past decade, ion chromatography (IC) has appeared as a contender with substantial benefits over established techniques. It is conducted without sample derivatization, unlike other techniques of comparable accuracy. Limits of detection (LOD) are also comparable, typically 20 μg/L when coupled with a pulsed amperometric detector or 1 mg/kg food using ion chromatography single quadrupole mass spectrometry. This compares to LODs of 2 g/kg food by high performance/liquid chromatography refractive index detector and 2 mg/kg food for gas chromatography/mass spectrometry. The main strength of ion chromatography is the specificity/differentiation of simple saccharides, that has resulted in the discoveries of several unreported saccharides in foods. Examples include isomaltose in flour, erlose in stingless bee honey and arabinose, ribose, rhamnose, xylose, mannose, trehalose, maltose and raffinose in paprika. Evolving future advantages of ion chromatography in saccharide analysis include the increasing utilization of mass spectrometry, more work towards a standardized analytical methodology, and the need to investigate new, novel and admixed food types so that instrumentation continues to demonstrate relevance at the cutting edge of food research.

Ephedrine remains a key precursor in the production of methamphetamine. A novel ephedrine-based route to methamphetamine involved the nitrosation of propiophenone to alpha-isonitrosopropiophenone, followed by catalytic hydrogenation to phenylpropanolamine (+/-- norephedrine). Cyclization-methylation of phenylpropanolamine to 3,4-dimethyl-5-phenyl-2-oxazolidinone using dimethyl carbonate, followed by basic hydrolysis or catalytic hydrogenolysis formed ephedrine or methamphetamine, respectively. An investigation into the stable isotope fractionation during the synthesis of methamphetamine from propiophenone, NaNO2 and dimethyl carbonate was performed using isotope ratio mass spectrometry. A negative isotopic shift was observed for S15N upon nitrosation of propiophenone to alpha-isonitrosopropiophenone, and a negative isotopic shift for S2H during catalytic hydrogenation of alpha-isonitrosopropiophenone to phenylpropanolamine. Minimal change in S13C was observed throughout the reaction until the methylation step with dimethyl carbonate, where a negative isotopic shift was observed. The S13C values for the methamphetamine presented in a similar range to methamphetamine reported in previous work where the norephedrine/norpseudoephedrine was prepared via different starting materials (benzaldehyde and nitroethane), confirming that similar S13C values will result from fractionation during methylation with dimethyl carbonate regardless of the origin of the norephedrine/norpseudoephedrine. Chiral analysis confirmed methamphetamine to be racemic.

The Forensic Isotope Ratio Mass Spectrometry (FIRMS) Network announce the publication of the Third Edition of the Good Practice Guide for Isotope Ratio Mass Spectrometry. In the third edition, changes include a new chapter on sampling covering method of sampling a population, sampling for homogeneity testing of a material as well as considerations for measurement uncertainty arising from sampling. The measurement uncertainty section has been revised and expanded to touch on alternative methods to combine uncertainty components together. Methods for measurement of water isotopic composition using equilibration have also been added. Additional detail has been included to expand on topics such as the difference between a reference gas and a working gas, additional tests that might be performed to check instrumental performance and initial data processing such as peak identification amongst others.

Traditional forensic chemical comparisons of polymeric materials are often affected by fingerprinting agents that enhance and visualise finger-marks. This can inhibit detailed analysis used to provide an association or discrimination between two samples. In this study, we have demonstrated that the method for polymer comparisons using isotope ratio mass spectrometry analysis is not affected by fingerprinting matter on the surface in contrast to other forensic instrumental tests. A selection of resealable bags was analysed for carbon and hydrogen isotope ratio values of bags that had been subject to various fingerprinting agents and compared to values of untreated bags. The results showed no significant difference between samples that had been fingerprinted from those that were untreated.

In previous work, a novel pathway for the synthesis of ephedrine/pseudoephedrine and methamphetamine using the precursors benzaldehyde, nitroethane and dimethyl carbonate was investigated, and an impurity profile presented. This paper presents chiral and stable isotope ratios of ephedrine/pseudoephedrine and methamphetamine synthesised by this pathway. Based on the chiral profile and the more negative 8 13 C (avg. -33.2%0) and more positive 8 2 H values, it is possible to distinguish ephedrine/pseudoephedrine and methamphetamine prepared from this pathway from those of "fully synthetic ", "semi-synthetic " or "natural " origin. The more positive 8 2 H values of methamphetamine from this pathway allowed for differentiation from methamphetamine produced from phenyl-2-propanone. It was noted, however, that the use of stable isotope profiling would likely be limited when a benzaldehyde source having a negative 8 2 H value was used as a precursor. Furthermore, the stable isotope values alone could not be used to differentiate from methamphetamine prepared by the AkaboriMomotani reaction, highlighting the need for combination with impurity profiling.

In the wake of recent, highly publicized examples of anti-Black racism, scholars and practitioners are seeking ways to use their skills, resources, and platforms to better understand and address this phenomenon. Naming, examining, and countering anti-Black racism are critical steps toward fostering antiracist science and practice. To support those efforts, this paper details key insights from past research on anti-Black racism in organizations, draws from critical race perspectives to highlight specific topics that warrant consideration in future research, and offers considerations for how scholars should approach anti-Black racism research. Future research ideas include: specific manifestations of anti-Black racism within organizations, the double-bind of authenticity for Black employees, intersectionality among Black employees, and means of redressing anti-Black racism in organizations. Suggested research considerations include: understanding the history of anti-Black racism within research and integrating anti-Black racism research insights across organizational science. Research insights, ideas, and considerations are outlined to provide context for past and current experiences and guidance for future scholarship concerning anti-Black racism in organizations.

Despite differences in their overall metabolism, eukaryotes share a common mitochondrial biochemistry. We investigated how this fundamental biochemistry supports overall metabolism using a high-resolution carbon isotope approach, position-specific isotope analysis. We measured carbon isotope 13C/12C cycling in animals, focusing on amino acids that are formed in mitochondrial reactions and are most metabolically active. Carboxyl isotope determinations for amino acids showed strong signals related to common biochemical pathways. Contrasting isotope patterns were measured for metabolism associated with major life history patterns, including growth and reproduction. Turnover of proteins and lipids as well as gluoconeogensis dynamics could be estimated for these metabolic life histories. The high-resolution isotomics measurements fingerprinted metabolism and metabolic strategies across the eukaryotic animal kingdom, yielding results for humans, ungulates, whales, and diverse fish and invertebrates in a nearshore marine food web.

In 2017 Cooktown resident Donna Steele was murdered and the case remained unsolved for more than a year. The forensic evidence from the investigation included two lengths of synthetic twine and a new protocol for the comparison of twine was developed to enhance the potential value of any evidence. The method was developed using 23 samples of similar twine collected across Australia. Traditional methods of physical and microscopic comparisons and polymer analysis by infrared spectroscopy were retained. Micro-spectrophotometry was used as an objective assessment of colour and was able to identify five groupings within the background samples. Measurements of hydrogen and carbon stable isotopic composition provided further delineation of the background samples. Combining traditional methods with micro-spectrophotometry and stable isotope measurements, the two case samples were found to be distinct from the background population and were indistinguishable when compared to each other.

The forensic comparative analysis of cling films often lacks the capability to discriminate samples to the level required for court purposes. Isotope ratio mass spectrometry (IRMS) can be used in addition to the traditional forensic analysis to add further discrimination to soft polymers such as cling films. Seventy one cling films purchased from around Australia and three sent from overseas were used to determine the variability of isotopic compositions in polyethylene cling films from Australia and to create a background database, useful for identifying the strength of comparisons. These were all analysed using Fourier Transform Infrared (FTIR) and IRMS and the results showed that FTIR analysis could discriminate 73% whilst IRMS can discriminate 95% of cling films. This study demonstrates how IRMS can be applied to the differentiation and sourcing of cling films if associated with a crime in Australia.

RationaleStable isotopic ratios can provide information for illicit drug profiling. The research presented here investigated the variations in stable isotopic ratios of hydrogen (δ2H), carbon (δ13C), nitrogen (δ15N) and oxygen (δ18O) during the synthesis of MDP2P (3,4‐methylenedioxyphenyl‐2‐propanone) and MDA (3,4‐methylenedioxyamphetamine) prepared via the ‘nitrostyrene’ route.MethodsSamples of MDA and MDP2P were synthesised from two isotopically characterised starting materials, piperonal and nitroethane. The isotopic compositions of the nitrostyrene intermediate (3,4‐methylenedioxyphenyl‐2‐nitropropene, MDP2NP) and products MDP2P and MDA were also measured by isotope ratio mass spectrometry.ResultsA significantly negative change occurred to δ2H values during the production of MDP2NP, MDP2P and MDA, indicating a mechanism that favours inclusion or retention of 1H over 2H. This suggests that the δ2H compositions of MDA/MDP2P prepared from piperonal will not provide information on the synthetic history. Minimal changes were observed in δ13C composition during the synthesis of MDP2NP, MDP2P and MDA, and minimal δ15N compositional changes occurred in MDP2NP and MDA. Progressing from piperonal to MDP2NP, a minimal change occurred to δ18O composition. A variable change to δ18O was observed from MDP2NP with one sample becoming more positive in δ18O composition and two samples becoming more negative. Progressing from MDP2NP to MDA, a significant negative change occurred to δ18O composition.ConclusionsThe changes to stable isotopic ratios observed during the preparation of MDA and MDP2P from piperonal may prove useful when attempting to compare batch‐to‐batch variations between seizures and provide information with tactical intelligence applications.

•Foundational review paper on amino acid analysis by Ion Chromatography of food.•Most Ion Chromatography methodology references one seminal paper.•No methodology found for analysis by Ion Chromatography mass spectrometry in food.•ICMS is an evolving area with no methodology for amino acids in food.•Advantages of Ion Chromatography analysis of amino acids.

An investigation into isotopic fractionation during the production of 3,4-methylenedioxymethylamphetamine (MDMA) from the novel precursor helional, and during the hydrochloric (HCl) salt precipitation of MDMA was conducted. Minimal changes occurred to delta C-13 composition from helional to MDMA.HCl. Isotope fractionation was, however, observed in delta H-2, delta O-18 and delta N-15 compositions. These results suggest minimal information with strategic intelligence applications can be collected for MDMA by IRMS alone. However, information with tactical intelligence applications can be gained by identifying batch-to-batch variations between MDMA samples based on the isotopic changes observed here.From helional to 3,4-methylenedioxyphenyl-2-propanone (MDP2P) shifts were observed in delta H-2 and delta O-18 composition. Additional changes occurred to delta H-2 and delta O-18 compositions during the synthesis of MDMA from MDP2P. A positive shift was observed in delta N-15 composition from methylamine to MDMA during reductive amination of MDP2P. During the HCl salt precipitation of MDMA, fractionation of delta N-15 from xylene was consistent with the proposed mechanism. Smaller fractionation was observed from dichloromethane (DCM). Fractionation also occurred to delta H-2 compositions during HCl salt precipitation which is explained by the addition of hydrogen during the process.

Presented here is an investigation into the stable isotopic ratios of 3,4-methylenedioxyamphetamine (MDA) prepared from the alternative precursor helional. Two methods for the synthesis of MDA were investigated, both utilising hydroxylamine as the nitrogen source. Recent publications found both helional and hydroxylamine with isotopic compositions significantly different to traditional precursors and nitrogen sources. While minimal fractionation was observed in carbon isotopic compositions, apparent fractionation occurred to hydrogen, ni-trogen and oxygen isotopic compositions during the synthesis of MDA. Fractionation observed in delta N-15 were explained by the reaction conditions during the addition of hydroxylamine. The fractionation observed in delta O-18 was consistent with the replacement and loss of an oxygen atom during the synthesis of the amide intermediate and MDA. A brief investigation into isotopic fractionation during MDA hydrogen chloride (HCl) salt precipitation was also conducted, and additional fractionation may be expected in both delta H-2 and delta N-15 during the process, consistent with the proposed mechanism. These results suggest that tactical intelligence can be gained from the batch-to-batch variations to isotopic composition of MDA during the synthesis from helional.

RATIONALEStable isotopic ratios can provide information for illicit drug profiling. The research presented here investigated the variations in stable isotopic ratios of hydrogen (δ2 H), carbon (δ13 C), nitrogen (δ15 N) and oxygen (δ18 O) during the synthesis of MDP2P (3,4-methylenedioxyphenyl-2-propanone) and MDA (3,4-methylenedioxamphetamine) prepared via the 'nitrostyrene' route.METHODSamples of MDA and MDP2P were synthesised from two isotopically characterised starting materials, piperonal and nitroethane. The isotopic composition of the nitrostyrene intermediate (3,4-methylenedioxyphenyl-2-nitropropene, MDP2NP) and products MDP2P and MDA were also measured by isotope ratio mass spectrometry (IRMS).RESULTSA significantly negative change occurred to δ2 H values during the production of MDP2NP, MDP2P and MDA, indicating a mechanism that favours inclusion or retention of 1 H over 2 H. This suggests that the δ2 H compositions of MDA/MDP2P prepared from piperonal will not provide information on the synthetic history. Minimal changes were observed in δ13 C composition during the synthesis of MDP2NP, MDP2P and MDA, and minimal δ15 N compositional changes occurred in MDP2NP and MDA. Progressing from piperonal to MDP2NP a minimal change occurred to δ18 O composition. A variable change to δ18 O was observed from MDP2NP with one sample becoming more positive in δ18 O composition and two samples becoming more negative Progressing from MDP2NP to MDA a significant negative change occurred to δ18 O composition.CONCLUSIONSThe changes to stable isotopic ratios observed during the preparation of MDA and MDP2P from piperonal may prove useful when attempting to compare batch-to-batch variations between seizures and provide information with tactical intelligence applications.

Abstract Stable hydrogen, carbon, nitrogen, oxygen and sulfur (HCNOS) isotope compositions expressed as isotope-delta values are typically reported relative to international standards such as Vienna Standard Mean Ocean Water (VSMOW), Vienna Peedee belemnite (VPDB) or Vienna Cañon Diablo Troilite (VCDT). These international standards are chosen by convention and the calibration methods used to realise them in practice undergo occasional changes. To ensure longevity and reusability of published data, a comprehensive description of (1) analytical procedure, (2) traceability, (3) data processing, and (4) uncertainty evaluation is required. Following earlier International Union of Pure and Applied Chemistry documents on terminology and notations, this paper proposes minimum requirements for publishing HCNOS stable-isotope delta results. Each of the requirements are presented with illustrative examples.

Hexamine, derived from solid fuel tablets, is a potential source for a number of home-made explosives including the primary high explosive hexamethylene triperoxide diamine (HMTD). Therefore, a means to characterise hexamine samples and to link HMTD with precursor hexamine may provide investigative intelligence to counter-terrorism agencies.We report the hydrogen, carbon and nitrogen isotopic compositions of hexamine isolated from retail samples of solid fuel tablets. Hydrogen isotopic compositions ranged from -123.0 to +172.6%o, carbon isotopic com-positions from -47.1 to -27.6%o and nitrogen isotopic compositions from -3.1 to +0.3%o. Despite within-and between-tablet inhomogeneity, a combination of these data could be considered characteristic of specific brands or manufacturers. Ten samples of hexamine were each used to synthesize four batches of HMTD using two isotopically distinct sources of hydrogen peroxide. The delta 13C and delta 15N compositions of the HMTD ranged from -48.8 to -31.5%o for carbon and from +13.7 to +17.8%o for nitrogen. delta 2H compositions across all batches of HMTD was much wider than previously reported; -109.3 to +196.6%o. The changes in carbon and nitrogen isotopic compositions, progressing from hexamine to HMTD, could be explained by a reaction mechanism involving the decomposition of hexamine to methylimine and formaldehyde. Data also supported a mechanism whereby the hydrogen atoms of HMTD were derived from hexamine and not from other reagents.Based on the relationships Delta 2HHEXAMINE-HMTD and Delta 13CHEXAMINE-HMTD, a rule-of-thumb was proposed to identify possible hexamine precursors of HMTD.