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ToF-SIMS characterisation of diterpenoic acids after chromatographic separation

机译：色谱分离后二萜酸的ToF-SIMS表征

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摘要

Microcolumn liquid chromatography (mu HPLC) coupled on-line with time of flight secondary ion mass spectrometry (ToF-SIMS) was applied for mixture of diterpenoic acids (abietic, gibberellic and kaurenoic) analysis. Chromatographic effluent, with analytes separated, was carried out directly onto different, ToF-SIMS compatible surface substrates, for further ToF-SIMS analysis. Silica gel Si-60, aluminium backplate modified Si-60, monolithic silica gel and Raman spectroscopy chromatographic thin layers were used as the deposition substrates in this experiment. By ToF-SIMS surface imaging the deposition trace picture has been obtained. Effluent deposition surface area was scanned for diterpenoic acid fragment mass values based on mass spectrometric library. Measured ToF-SIMS dataset of fragment abundance and intensities were used for preliminary fragmentation schemes construction. The lowest substrate background activity has been established for monolithic silica gel thin layer and aluminium backplate modified Si-60 thin layer. In the case of Raman spectroscopy pre-treated thin layer or conventional chromatographic thin layer Si-60, the both, high background signal intensity and impossibility to construct negative ions surface image, were observed. Diterpenoic acids studied serve the similar mass spectrum but ToF-SIMS coupled with liquid chromatographic separation brings new impact to the positive identification of analytes studied. (c) 2006 Elsevier B.V. All rights reserved.
机译：在线联用飞行时间二次离子质谱（ToF-SIMS）的微柱液相色谱（μHPLC）用于二萜酸的混合物（松香酸，赤霉素和脲醛酸）分析。分离出分析物的色谱流出物直接在不同的，与ToF-SIMS兼容的表面基质上进行，以进行进一步的ToF-SIMS分析。硅胶Si-60，铝背板改性的Si-60，整体硅胶和拉曼光谱层析薄层用作本实验的沉积基质。通过ToF-SIMS表面成像，获得了沉积轨迹图。根据质谱库扫描废水沉积表面积的二萜酸片段质量值。测得的片段丰度和强度的ToF-SIMS数据集用于初步片段化方案的构建。对于整体硅胶薄层和铝背板改性的Si-60薄层，已经确定了最低的底物背景活性。在拉曼光谱法预处理的薄层或常规色谱薄层Si-60的情况下，观察到高背景信号强度和无法构造负离子表面图像两者。所研究的二萜酸具有相似的质谱，但是ToF-SIMS与液相色谱分离相结合对所分析物的阳性鉴定产生了新的影响。 （c）2006 Elsevier B.V.保留所有权利。

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