Mass spectrometric analysis of sulfur in microgram quantities of biological macromolecules using a reaction interface.
Mass spectrometric analysis of sulfur in microgram quantities of biological macromolecules using a reaction interface.
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使用反应接口对微克量的生物大分子中的硫进行质谱分析。
DOI：
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发表时间：
1986
期刊：
影响因子：
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通讯作者：
S. Markey
中科院分区：
文献类型：
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作者：
F. Abramson;S. Markey
使用反应界面和质谱仪对各种蛋白质的亚微克到微克样品进行了分析。界面在微波放电中雾化大分子，并通过与清道夫气体反应，从分析物中包含的元素生成简单的多原子分子。在二氧化碳清除放电中，SO2的m/z的测量可以用来确定最初引入界面的硫量；在氮气清除放电中，碳被定量为HCN(m/z 27)。由于反应界面的高能、破坏性性质，原始分子的性质，即大小、极性等，不影响分析，只影响其元素含量。一系列12种氨基酸聚合物的样品(1微克)，大小从摩尔数不等。WT 470(DES-TYR-MET-脑啡肽)。对牛血清白蛋白(WT 65,400)和硫含量为1 S/氨基酸(聚-1-蛋氨酸)至2 S/153氨基酸(肌红蛋白)的蛋白质进行了硫和碳的元素分析。观测到的S/碳比值与元素式计算呈线性关系，对数-对数回归系数为0.80。与聚-1-蛋氨酸(摩尔.WT 30 000)作为模型化合物，硫的检出量在20~10 000 ng范围内呈线性关系。我们得出的结论是，该反应界面是一种很有前途的补充，用于从生物大分子的小样本中检测某些元素的质谱计。
Submicrogram to microgram samples of a variety of proteins have been analyzed using a reaction interface and a mass spectrometer. The interface atomizes the macromolecule in a microwave discharge and produces simple polyatomic molecules from the elements contained in the analyte by reaction with a scavenger gas. The measurement of m/z 64 for SO2 in a CO2-scavenged discharge can be used to determine the amount of sulfur originally introduced into the interface; carbon is quantified as HCN (m/z 27) in a nitrogen-scavenged discharge. Because of the highly energetic, destructive nature of the reaction interface, the character of the original molecule, i.e. size, polarity, etc., does not affect the analysis, only its elemental content. Samples (1 microgram) of a series of 12 amino acid polymers ranging in size from mol. wt 470 (des-TYR-MET-enkephalin) to mol. wt 65,400 (bovine serum albumin) and with a sulfur content of 1 S per amino acid (poly-1-methionine) to 2 S per 153 amino acids (myoglobin) were subjected to elemental analyses of sulfur and carbon. The observed S/C ratio was linear with elemental formula calculation, and produced a log-log regression coefficient of 0.80. With poly-1-methionine (mol. wt 30 000) as a model compound, the detection of sulfur was linear for sample sizes between 20 and 10 000 ng. We conclude that the reaction interface is a promising addition to a mass spectrometer for detection of certain elements from small samples of biological macromolecules.