Extraction and Isotope Measurement of Sulfur in Biological Samples

Extraction and Isotope Measurement of Sulfur in Biological Samples
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生物样品中硫的提取和同位素测量

DOI:
10.2116/analsci.3.157
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发表时间:
1987
期刊:
影响因子:
--
通讯作者:
A. Sasaki
A. Sasaki
中科院分区:
--
文献类型:
--
作者:
Y. Arikawa;A. Sasaki

文献摘要

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研究了一种从生物样品中完全提取硫的方法,以辅助生物硫的同位素测定。样品在高压氧气下燃烧。形成的三氧化硫被吸收在水中,以硫酸钡的形式固定下来,然后用锡(II)-强磷酸(将二水合氯化锡溶解在浓缩的正磷酸中制成的试剂)加热。通过该过程形成的硫化氢进一步转化为硫化银。同位素比值按常规方法以δ ^34S % ‰表示,即,硫化银与氧化铜(I)的燃烧,形成的二氧化硫的连续真空蒸馏,以及通过质谱仪测量其同位素比。通过重复分析胱氨酸和蛋氨酸作为含硫样品,在每个阶段仔细检查整个过程。尝试了测量指甲和头发样本中硫的同位素组成的初步应用。
A method to extract sulfur completely from biological samples was investigated to assist the isotopic measurement of biosulfur. A sample is burnt under a high pressure of oxygen. The sulfur trioxide formed is absorbed in water to fix it as barium sulfate, which in turn is heated with tin(II)-strong phosphoric acid (the reagent made by dissolving tin(II) chloride dihydrate in condensed orthophosphoric acid). The hydrogen sulfide formed by this procedure is further transformed into silver sulfide. The isotopic ratio is obtained in terms of δ^34S%‰ according to the conventional method, i.e., combustion of silver sulfide with copper(I) oxide, successive vacuum distillation of formed sulfur dioxide, and measurement of its isotopic ratio by a mass spectrometer. The whole procedure was carefully examined at each stage by repeated analyses of cystine and methionine as sulfur-containing samples. Preliminary applications to measure the isotopic composition of sulfur in nail and hair samples were attempted.