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对保存在考古骨骼和牙齿中的胆固醇进行的δ¹³C分析。

delta 13C analysis of cholesterol preserved in archaeological bones and teeth.

作者信息

Stott A W, Evershed R P

机构信息

Organic Geochemistry Unit, School of Chemistry, University of Bristol, U.K.

出版信息

Anal Chem. 1996 Dec 15;68(24):4402-8. doi: 10.1021/ac960199r.

Abstract

Cholesterol preserved in archaeological bones and teeth constitutes an important new source of palaeodietary information. A method is described here for the isotopic (delta 13C) determination of cholesterol employing a semiautomated sample preparation procedure and the technique of isotope ratio monitoring/gas chromatography/ mass spectrometry (irm/GC/MS). High-temperature gas chromatography (HT-GC) and high-temperature gas chromatography/mass spectrometry (HT-GC/MS) were used to identify the lipids and quantify the cholesterol present in the total lipid extracts. delta 13C values are then readily obtained from nanogram amounts (approximately 50 ng) of cholesterol resolved and determined directly by high-resolution capillary irm/GC/MS of trimethylsilylated total lipid extracts. The protocol developed allows effective processing of the large numbers of samples essential for palaeodietary determinations. Analytical precision and reproducibility have been assessed through multiple sampling of the same skeleton (femur, 9th century). Comparable delta 13C values have been obtained from different skeletal members from the same individual. The utility of the approach is demonstrated through a study of the delta 13C values of cholesterol isolated from sections of femoral bones of individuals excavated from cemeteries (dated Saxon to 18th century) at a coastal site in the U.K. The mean delta 13C value (-22.2 +/- 0.3/1000, sigma = 0.9) determined for cholesterol in 50 different individuals indicates a strong preference for marine foods by the members of the community extending back over the last approximately 1500 years. A minority of individuals exhibited delta 13C values as low as -26/1000, indicating preferences for terrestrial rather than marine foodstuffs.

摘要

保存在考古骨骼和牙齿中的胆固醇构成了古饮食信息的一个重要新来源。本文描述了一种采用半自动样品制备程序以及同位素比率监测/气相色谱/质谱技术(irm/GC/MS)来测定胆固醇同位素(δ¹³C)的方法。高温气相色谱(HT-GC)和高温气相色谱/质谱(HT-GC/MS)用于鉴定脂质并定量总脂质提取物中存在的胆固醇。然后,通过对三甲基硅烷基化总脂质提取物进行高分辨率毛细管irm/GC/MS直接解析并测定纳克量(约50纳克)的胆固醇,可轻松获得δ¹³C值。所开发的方案能够有效地处理古饮食测定所需的大量样品。通过对同一具骨骼(9世纪股骨)进行多次采样评估了分析精度和重现性。从同一个体的不同骨骼部位获得了可比的δ¹³C值。通过对从英国沿海一处墓地(年代从撒克逊时期到18世纪)发掘出的个体股骨切片中分离出的胆固醇的δ¹³C值进行研究,证明了该方法的实用性。对50个不同个体的胆固醇测定的平均δ¹³C值(-22.2±0.3‰,σ = 0.9)表明,在过去约1500年里,该社区成员强烈偏好海洋食物。少数个体的δ¹³C值低至-26‰,表明他们偏好陆地而非海洋食物。

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