Purification of dinosterol for hydrogen isotopic analysis using high-performance liquid chromatography-mass spectrometry.

Purification of dinosterol for hydrogen isotopic analysis using high-performance liquid chromatography-mass spectrometry.
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使用高效液相色谱-质谱法纯化地甾醇用于氢同位素分析。

DOI:
10.1016/j.chroma.2007.09.018
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发表时间:
2007
期刊:
Journal of chromatography. A
影响因子:
--
通讯作者:
J. Sachs
J. Sachs
中科院分区:
--
文献类型:
--
作者:
R. Smittenberg;J. Sachs

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建立了一种半制备正相高效液相色谱-质谱(HPLC-MS)联用技术,用于沉积物总脂提取物中各种醇组分的分离纯化,并用于气相色谱-同位素比值质谱(GC-IRMS)氢同位素测定。4-甲基甾醇,包括甲藻特异性标志物甲藻甾醇(4,23,24-三甲基胆甾烷-22-烯-3 β-醇),成功地从臭名昭著的共洗脱植物衍生的五环三萜醇和烷基醇中分离。我们发现,大量的氢同位素分馏发生在色谱分离,证明了恢复整个峰时,随后的氢同位素分析进行的重要性。这是第一次报告,这样的氢同位素分馏天然未标记的化合物。
A semi-preparative normal-phase high-performance liquid chromatography–mass spectrometry (HPLC–MS) method is presented for the purification of various alcohol fractions from total lipid extracts derived from sediments, for the purpose of hydrogen isotopic measurement by gas chromatography–isotope ratio mass spectrometry (GC–IRMS). 4-Methylsterols, including the dinoflagellate-specific marker dinosterol (4,23,24-trimethylcholestan-22-en-3β-ol), were successfully separated from notoriously co-eluting plant-derived pentacyclic triterpenoid alcohols and alkyl alcohols. We find that substantial hydrogen isotope fractionation occurs during chromatographic separation, demonstrating the importance of recovering the entire peak when subsequent hydrogen isotope analyses are to be performed. This is the first report of such hydrogen isotopic fractionation for a natural unlabelled compound.
DOI: 10.1016/j.gca.2004.06.004
发表时间: 2004-12
影响因子: 5
作者:
D. Sachse;J. Radke;G. Gleixner
通讯作者: D. Sachse;J. Radke;G. Gleixner
DOI: 10.1038/nature03945
发表时间: 2005-10-13
期刊: NATURE
影响因子: 64.8
作者:
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通讯作者: Schneider, RR
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发表时间: 1997
期刊: Journal of chromatography. A
影响因子: --
作者:
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