Recent Advances in the Application of Stable Isotope Ratio Analysis in Forensic Chemistry

Daéid, Niamh Nic; Buchanan, Hilary A. S.; Savage, Katy; Fraser, James G.; Cresswell, Sarah L.

doi:10.1071/ch09414

Cited by 26 publications

(12 citation statements)

References 36 publications

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“…The natural isotopic variability of light elements, such as C, N, O, S, and H, indicate the geographic, chemical, and biological origins of substances and is of interest in a large cross-section of scientific disciplines 7, 8 , such as source identification 9 in ecology 10 , food authentication 11 , archaeology 12 , geochemistry 13 , environmental contaminants 14 , air pollution 15 , forensic sciences 16 , and as non-radioactive tracers in biomedical applications 17 . High precision gas isotope ratio mass spectrometry (IRMS) is used for the measurement of small differences in the stable isotopic abundances as a ratio in the sample relative to that in a traceable standard.…”

Section: Introductionmentioning

confidence: 99%

Detection of Synthetic Testosterone Use by Novel Comprehensive Two-Dimensional Gas Chromatography Combustion–Isotope Ratio Mass Spectrometry

et al. 2011

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We report the first demonstration of Comprehensive Two-dimensional Gas Chromatography Combustion Isotope Ratio Mass Spectrometry (GC×GCC-IRMS) for the analysis of urinary steroids to detect illicit synthetic testosterone use, of interest in sport doping. GC coupled to IRMS (GCC-IRMS) is currently used to measure the carbon isotope ratios (CIR, δ13C) of urinary steroids in anti-doping efforts; however, extensive cleanup of urine extracts is required prior to analysis to enable baseline separation of target steroids. With its greater separation capabilities, GC×GC has the potential to reduce sample preparation requirements and enable CIR analysis of minimally processed urine extracts. Challenges addressed include on-line reactors with minimized dimensions to retain narrow peaks shapes, baseline separation of peaks in some cases, and reconstruction of isotopic information from sliced steroid chromatographic peaks. Difficulties remaining include long-term robustness of on-line reactors and urine matrix effects that preclude baseline separation and isotopic analysis of low concentration and trace components. In this work, steroids were extracted, acetylated, and analyzed using a refined, home-built GC×GCC-IRMS system. 11-hydroxy-androsterone (11OHA) and 11-ketoetiocolanolone (11KE) were chosen as endogenous reference compounds (ERC) because of their satisfactory signal intensity, and their CIR was compared to target compounds (TC) androsterone (A) and etiocholanolone (E). Separately, a GC×GC-qMS system was used to measure testosterone (T)/EpiT concentration ratios. Urinary extracts of urine pooled from professional athletes, and urine from one individual that received testosterone gel (T-gel) and one individual that received testosterone injections (T-shot) were analyzed. The average precisions of δ13C and Δδ13C measurements were SD(δ13C) approximately ± 1‰ (n=11). The T-shot sample resulted in a positive for T use with a T/EpiT ratio of > 9 and CIR measurements of Δδ13C > 5‰, both fulfilling World Anti-Doping Agency criteria. These data show for the first time that synthetic steroid use is detectable by GC×GCC-IRMS without need for extensive urine cleanup.

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Section: Introductionmentioning

confidence: 99%

Detection of Synthetic Testosterone Use by Novel Comprehensive Two-Dimensional Gas Chromatography Combustion–Isotope Ratio Mass Spectrometry

et al. 2011

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“…An interesting tool for studying such links is isotope ratio mass spectrometry (IRMS), as this technique has the potential to differentiate between chemically identical substances based on differences in their isotopic composition. IRMS techniques emerging from geological sciences in recent years quickly gained popularity in the forensic domain also because isotopic composition is often determined by geographic origin allowing provenancing .…”

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confidence: 99%

The Potential of Isotope Ratio Mass Spectrometry (IRMS) and Gas Chromatography‐IRMS Analysis of Triacetone Triperoxide in Forensic Explosives Investigations

Bezemer

Koeberg

Heijden

et al. 2016

Journal of Forensic Sciences

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Studying links between triacetone triperoxide (TATP) samples from crime scenes and suspects can assist in criminal investigations. Isotope ratio mass spectrometry (IRMS) and gas chromatography (GC)-IRMS were used to measure the isotopic compositions of TATP and its precursors acetone and hydrogen peroxide. In total, 31 TATP samples were synthesized with different raw material combinations and reaction conditions. For carbon, a good differentiation and a linear relationship were observed for acetone-TATP combinations. The extent of negative (δ(13) C) fractionation depended on the reaction yield. Limited enrichment was observed for the hydrogen isotope (δ(2) H) values of the TATP samples probably due to a constant exchange of hydrogen atoms in aqueous solution. For oxygen (δ(18) O), the small isotopic range and excess of water in hydrogen peroxide resulted in poor differentiation. GC-IRMS and IRMS data were comparable except for one TATP sample prepared with high acid concentration demonstrating the potential of compound-specific isotope analysis. Carbon IRMS has practical use in forensic TATP investigations.

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“…Various physical, chemical, and biological fractionation processes cause localized fractionation of different isotopes and the analysis of the resulting isotopes provenance of different materials. Several reviews have discussed forensic applications of IRMS (105)(106)(107)(108), and Meier-Augenstein (109) provided even more comprehensive coverage in his recent book Stable Isotope Forensics. In forensic applications, isotope ratio analysis provides information about the natural or synthetic origins of scheduled drugs (110)(111)(112)(113)(114)(115)(116)(117)(118)(119)(120), organic and inorganic explosives (76,121,122), petroleum hydrocarbons (such as in ignitable liquids) (65,66,(123)(124)(125)(126), and various other forensic materials (such as fibers, matches, and paint chips) (127)(128)(129)(130)(131).…”

Section: Stable Isotope Analysismentioning

confidence: 99%

Forensic Mass Spectrometry

Hoffmann¹,

Jackson

2015

Annual Rev. Anal. Chem.

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Developments in forensic mass spectrometry tend to follow, rather than lead, the developments in other disciplines. Examples of techniques having forensic potential born independently of forensic applications include ambient ionization, imaging mass spectrometry, isotope ratio mass spectrometry, portable mass spectrometers, and hyphenated chromatography-mass spectrometry instruments, to name a few. Forensic science has the potential to benefit enormously from developments that are funded by other means, if only the infrastructure and personnel existed to adopt, validate, and implement the new technologies into casework. Perhaps one unique area in which forensic science is at the cutting edge is in the area of chemometrics and the determination of likelihood ratios for the evaluation of the weight of evidence. Such statistical techniques have been developed most extensively for ignitable-liquid residue analyses and isotope ratio analysis. This review attempts to capture the trends, motivating forces, and likely impact of developing areas of forensic mass spectrometry, with the caveat that none of this research is likely to have any real impact in the forensic community unless: (a) The instruments developed are turned into robust black boxes with red and green lights for positives and negatives, respectively, or (b) there are PhD graduates in the workforce who can help adopt these sophisticated techniques.

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Recent Advances in the Application of Stable Isotope Ratio Analysis in Forensic Chemistry

Cited by 26 publications

References 36 publications

Detection of Synthetic Testosterone Use by Novel Comprehensive Two-Dimensional Gas Chromatography Combustion–Isotope Ratio Mass Spectrometry

Detection of Synthetic Testosterone Use by Novel Comprehensive Two-Dimensional Gas Chromatography Combustion–Isotope Ratio Mass Spectrometry

The Potential of Isotope Ratio Mass Spectrometry (IRMS) and Gas Chromatography‐IRMS Analysis of Triacetone Triperoxide in Forensic Explosives Investigations

Forensic Mass Spectrometry

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