Cheng Juan, Winograd Nicholas
Department of Chemistry, The Pennsylvania State University, 104 Chemistry Building, University Park, Pennsylvania 16802, USA.
Anal Chem. 2005 Jun 1;77(11):3651-9. doi: 10.1021/ac048131w.
A buckminsterfullerene ion source is employed to characterize peptide-doped trehalose thin films. The experiments are designed to utilize the unique sputtering properties of cluster ion beams for molecular depth profiling. The results show that trehalose films with high uniformity can be prepared on Si by a spin-coating technique. Bombardment of the film with C60+ results in high quality time-of-flight secondary ion mass spectrometry spectra, even during ion doses of up to 3 x 10(14) ions/cm2. This result is in contrast to atomic bombardment experiments in which the dose of incident ions must be kept below 10(12) ions/cm2 so as to retain mass spectral information. Moreover, since the films are of uniform thickness, it is possible to depth-profile through the film and into the Si substrate. This experimental protocol allows the yield of trehalose molecular equivalents and the degree of interface mixing to be evaluated in detail. When doped with a variety of small peptides up to a molecular weight of m/z 500, we find that the peptide molecular ion intensity remains stable under continuous C60+ bombardment, although some decrease in intensity is observed. The results are interpreted in terms of a model whereby the high trehalose yield and low damage depth of the C60 projectile combine to prevent damage accumulation. In general, the peptide-trehalose system provides a valuable model for evaluating the parameters that lead to effective 3-dimensional characterization of biomaterials.
采用巴克敏斯特富勒烯离子源对肽掺杂海藻糖薄膜进行表征。这些实验旨在利用团簇离子束独特的溅射特性进行分子深度剖析。结果表明,通过旋涂技术可在硅片上制备出具有高均匀性的海藻糖薄膜。用C60+轰击该薄膜能得到高质量的飞行时间二次离子质谱图,即使在离子剂量高达3×10(14)离子/cm2时也是如此。这一结果与原子轰击实验形成对比,在原子轰击实验中,入射离子剂量必须保持在10(12)离子/cm2以下,以保留质谱信息。此外,由于薄膜厚度均匀,有可能对薄膜及硅衬底进行深度剖析。这种实验方案能够详细评估海藻糖分子当量的产率和界面混合程度。当掺杂多种分子量高达m/z 500的小肽时,我们发现尽管观察到强度有所下降,但在连续的C60+轰击下,肽分子离子强度仍保持稳定。这些结果根据一个模型进行解释,即C60弹丸的高海藻糖产率和低损伤深度相结合可防止损伤积累。总体而言,肽 - 海藻糖体系为评估导致生物材料有效三维表征的参数提供了一个有价值 的模型。