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Semi‐online nanoflow liquid chromatography/matrix‐assisted laser desorption ionization mass spectrometry of synthetic polymers using an octadecylsilyl‐modified monolithic silica capillary column
Author(s) -
Watanabe Takehiro,
Nakanishi Keisuke,
Ozawa Tomoyuki,
Kawasaki Hideya,
Ute Koichi,
Arakawa Ryuichi
Publication year - 2010
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.4584
Subject(s) - chemistry , chromatography , monolithic hplc column , elution , column chromatography , mass spectrometry , desorption , analytical chemistry (journal) , capillary action , polymer , capillary electrochromatography , size exclusion chromatography , tetrahydrofuran , high performance liquid chromatography , materials science , adsorption , capillary electrophoresis , organic chemistry , composite material , enzyme , solvent
We have designed a semi‐online liquid chromatography/matrix‐assisted laser desorption/ionization mass spectrometry (LC/MALDI‐MS) system to introduce eluent from a octadecylsilyl (ODS) group modified monolithic silica capillary chromatographic column directly onto a sample plate for MALDI‐MS analysis. Our novel semi‐online system is useful for rapidly and sensitively examining the performance of a monolithic capillary column. An additional advantage is the small elution volume of a monolithic capillary column, which allows delicate eluents, such as 1,1,1,3,3,3,‐hexafluoroisopropyl alcohol (HFIP), to be used to achieve cost‐effective analysis. Using the semi‐online LC/MALDI‐MS system, chromatographic separation of polymers by the monolithic column with different eluents was studied. Separation of poly(methyl methacrylate) and Nylon 6/6 showed that the column functioned via size‐exclusion separation when tetrahydrofuran or HFIP eluent was used. On the other hand, the separation behavior of Nylon 11 indicated a reversed‐phase mode owing to the interaction of the polymer with the modified ODS group in the column. Using tetrahydrofuran/methanol (1:1, v/v) as the eluent, the LC/MALDI‐MS spectra of poly(lactic acid), which contains both linear and cyclic polymer structures, showed that the column could separate the hydrophobic cyclic polymer and elute it out relatively slowly. The monolithic column functions basically via size‐exclusion separation; the reversed‐phase separation by interaction with the ODS functions may have less influence on column separation. The semi‐online monolithic capillary LC/MALDI‐MS method we have developed should provide a means of effectively analyzing synthetic polymers. Copyright © 2010 John Wiley & Sons, Ltd.