A protocol for pressurized liquid extraction and processing methods to isolate modern and ancient bone cholesterol for compound‐specific stable isotope analysis

Laffey, Ann O.; Krigbaum, John; Zimmerman, Andrew R.

doi:10.1002/rcm.7786

Cited by 4 publications

(2 citation statements)

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“…So far, compound-specific isotope analysis (CSIA) by gas chromatography coupled to irm-MS [32,33] is the only method enabled to work with few milligrammes of products. None of the previously proposed irm-NMR approaches can cope with limitations regarding the cholesterol quantity and the NMR acquisition time.…”

Section: Introductionmentioning

confidence: 99%

A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR

et al. 2021

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Cholesterol, the principal zoosterol, is a key metabolite linked to several health complications. Studies have shown its potential as a metabolic biomarker for predicting various diseases and determining food origin. However, the existing INEPT (insensitive nuclei enhanced by polarization transfer) 13 C position-specific isotope analysis method of cholesterol by NMR was not suitable for very precise analysis of small quantities due to its long acquisition time and therefore is restricted to products rich in cholesterol. In this work, a symmetric and adiabatic heteronuclear single quantum coherence (HSQC) 2D NMR sequence was developed for the high-precision (few permil) analysis of small quantities of cholesterol. Adiabatic pulses were incremented for improving precision and sensitivity. Moreover, several strategies such as the use of non-uniform sampling, linear prediction, and variable recycling time were optimized to reduce the acquisition time. The number of increments and spectral range were also adjusted. The method was developed on a system with a cryogenically cooled probe and was not tested on a room-temperature system. Our new approach allowed analyzing as low as 5 mg of cholesterol in 31 min with a long-term repeatability lower than 2‰ on the 24 non-quaternary carbon atoms of the molecule comparing to 16.2 h for the same quantity using the existing INEPT method. This result makes conceivable the isotope analysis of matrices low in cholesterol.

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Section: Introductionmentioning

confidence: 99%

A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR

et al. 2021

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“…Lipid materials contain alcohols and sterols in addition to acylglycerols and wax esters. The characterization of lipid alcohols as sterols or hormones in sediments (Luong et al, 2018), bones (Charapata et al, 2018) or in teeth (Laffey, Krigbaum, & Zimmerman, 2017; Velsko et al, 2017), and the analysis of the unsaponifiable lipid fraction to obtain information of the source of fats and oils have also been reported (Mills & White, 1975). The analysis of hormones proved successful for the matrices enabling these biomolecules to survive burial, as is the case of bones.…”

Section: Introductionmentioning

confidence: 99%

Liquid chromatography and mass spectrometry for the analysis of acylglycerols in art and archeology

Nasa

Modugno

Degano

2020

Mass Spectrometry Reviews

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Lipid characterization in art and archeology, together with the study of lipid degradation processes, is an important research area in heritage science. Lipid‐based materials have been used as food since ancient times, but also employed as illuminants and as ingredients in cosmetic, ritual, and pharmaceutical preparations. Both animal and plant lipids have also been processed to produce materials used in art and crafts, such as paint binders, varnishes, waterproofing agents, and coatings. Identifying the origin of the lipid materials is challenging when they are found in association with artistic historical objects. This is due to the inherent complex composition of lipids, their widespread occurrence, and the chemical alterations induced by ageing. The most common approach for lipid characterization in heritage objects entails profiling fatty acids by gas chromatography/mass spectrometry after saponification or transesterification. New developments in high‐performance liquid chromatography coupled with mass spectrometry (HPLC‐MS) for the characterization of acylglycerols, together with more efficient sample treatments, have fostered the introduction of liquid chromatography for characterizing the lipid profile in heritage objects. This review reports the latest developments and applications of HPLC‐MS for the characterization of lipid materials in the field of heritage science. We describe the various approaches for sample pretreatment and highlight the advantages and limitations of HPLC‐MS in the analysis of paint and archeological samples. © 2020 John Wiley & Sons Ltd.

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Assessing the usefulness of Raman spectroscopy and lipid analysis of decomposed human bones in forensic genetics and molecular taphonomy

S.D. Corrêa,

Alessandri,

Verzeletti

2024

Forensic Science International

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A protocol for pressurized liquid extraction and processing methods to isolate modern and ancient bone cholesterol for compound‐specific stable isotope analysis

Abstract: These results should assist sample selection and provide an effective, alternative extraction method for bone cholesterol that may be used for isotopic and paleodietary analysis. Copyright © 2016 John Wiley & Sons, Ltd.

Cited by 4 publications

References 57 publications

A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR

A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR

Liquid chromatography and mass spectrometry for the analysis of acylglycerols in art and archeology

Assessing the usefulness of Raman spectroscopy and lipid analysis of decomposed human bones in forensic genetics and molecular taphonomy

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