Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry Chinese Academy of Sciences, Beijing 100190, China.
Anal Chem. 2011 Jul 1;83(13):5400-6. doi: 10.1021/ac200966m. Epub 2011 Jun 14.
This article reports an application of charge-detection quadrupole ion trap mass spectrometry (CD-ITMS) to characterize the column packing materials in high-performance liquid chromatography (HPLC). Both the mean mass and the mass distribution of the packing materials are obtained and used to calculate the specific surface area of unbonded silica, the carbon load of the bonded silica, and their particle size distributions. The obtained specific surface areas and carbon loads are consistent with those measured independently by nitrogen sorption and elemental analysis respectively, whereas the derived size distributions show better resolution than that measured by a laser particle size analyzer. Furthermore, we evaluate the uniformity of particle size, which is the key parameter for column efficiency of the liquid chromatography by analyzing the mass distribution of the packing materials at the top and bottom of the column. A broader mass distribution, which yields decreased column efficiency, is observed for the column top because of the excessive use of the column. Our results suggest that CD-ITMS can serve as an alternative means for the characterization of the packing materials in HPLC and is potentially useful for column quality control.
本文报道了电荷检测四极杆离子阱质谱（CD-ITMS）在高效液相色谱（HPLC）中柱填充材料表征方面的应用。获得了填充材料的平均质量和质量分布，并用于计算未键合硅胶的比表面积、键合硅胶的碳载量及其粒径分布。得到的比表面积和碳载量分别与氮吸附和元素分析独立测量得到的结果一致，而推导的粒径分布比激光粒度分析仪测量的结果具有更好的分辨率。此外，我们通过分析柱顶和柱底填充材料的质量分布来评估粒径的均匀性，这是液相色谱柱效率的关键参数。由于过度使用，柱顶的质量分布较宽，导致柱效率降低。我们的结果表明，CD-ITMS 可以作为 HPLC 中填充材料表征的替代手段，并且可能对柱质量控制有用。
