✦ LIBER ✦

Design, construction and application of a simple packed capillary high performance liquid chromatography/electrospray mass spectrometry system

✍ Scribed by Russell H. Robins; Jane E. Guido

Publisher: John Wiley and Sons
Year: 1997
Tongue: English
Weight: 162 KB
Volume: 11
Category: Article
ISSN: 0951-4198
DOI: 10.1002/(sici)1097-0231(19971015)11:15<1661::aid-rcm57>3.0.co;2-w

No coin nor oath required. For personal study only.

✦ Synopsis

A simple packed-capillary high performance liquid chromatography (HPLC) system for the analysis of trace (picogram) mixtures by electrospray mass spectrometry is described in detail. This simple and cost-effective design is constructed from conventional hardware generally available in the modern LC/MS laboratory. Short slurry-packed vitreous silica capillary columns (5 cm ؋ 200 µm i.d.) are prepared in minutes from a variety of commercial bulk packing materials by fast, medium pressure bomb packing. Precise submicroliter per minute gradient elution of the capillary column is achieved by precolumn flow splitting of a conventional, analytical-scale, gradient HPLC pump operating at 0.5 to 3.0 mL/min. flow rates. Chromatographic system dead volume is reduced to a minimum via unique integration of the splitter, injector, capillary column and electrospray emitter into a single assembly, thereby markedly improving chromatographic performance and ease of use. System performance is demonstrated through several applications, including the determination of caffeine in untreated urine, the analysis of tryptic peptide mixtures harvested from electrophoretic gels and the determination of trace impurities in pharmaceutical bulk drugs.

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