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一种用于纳升液相电喷雾串联质谱的单端锥形熔融石英填充毛细管柱的简单高效的 frit 制备方法。

A simple and efficient frit preparation method for one-end tapered-fused silica-packed capillary columns in nano-LC-ESI MS.

机构信息

Key Laboratory of Industrial Ecology and Environmental Engineering, Ministry of Education, School of Environmental Science & Technology, Dalian University of Technology, Dalian, PR China.

出版信息

Proteomics. 2010 Apr;10(8):1724-7. doi: 10.1002/pmic.200800736.

DOI:10.1002/pmic.200800736
PMID:20162556
Abstract

A novel frit preparation method for one-end tapered-fused silica-packed capillary columns in nano-LC-ESI MS was developed. A hollow-fused silica capillary column with a tapered tip as nano-spray emitter was filled with 5 microm C(18) beads, and then a sintered frit about 0.25 mm in length was prepared at the tip by butane flame. A stainless steel protection tube with 0.5 mm id was used to control the length of the frit and to protect the packed C(18) beads behind the sintered frit during the sintering. C(18) sintered frits were evaluated by BSA tryptic digests with nano-LC-LTQ. The sintered frits did not produce post-column band broadening due to very small volume (about 0.2 nL) and did not produce adsorption to sample. The sintered frit columns had good separation reproducibility and separation performance compared with self-assembled particles frit columns and commercial columns.

摘要

开发了一种用于纳升电喷雾-线性离子阱质谱的新型熔融石英毛细管柱一端锥形填充柱的制备方法。将具有锥形尖端的空心熔融石英毛细管柱填充 5 微米 C(18)珠子,然后在尖端用丁烷火焰制备约 0.25 毫米长的烧结滤片。使用内径为 0.5 毫米的不锈钢保护管来控制滤片的长度,并在烧结过程中保护烧结滤片后面的填充 C(18)珠子。用纳升 LC-LTQ 分析 BSA 酶切物来评估 C(18)烧结滤片。由于体积非常小(约 0.2 nL),烧结滤片不会导致柱后展宽,也不会对样品产生吸附。与自组装颗粒滤片柱和商业柱相比,烧结滤片柱具有良好的分离重现性和分离性能。

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