Analysis of boronic acids by nano liquid chromatography-direct electron ionization mass spectrometry.
A new method, based on a direct-electron ionization (EI) interface, is presented for the analysis of compounds insufficiently amenable to usual MS methods. The instrumentation is composed of a nano liquid chromatograph (LC) and a mass spectrometer (MS) directly coupled by a transfer capillary. The eluent is directly introduced into the heated electron impact ion source of the MS. Significant advantages are the generation of reproducible spectra and the ability to ionize highly polar compounds. Boronic acids are used as coupling reagents to produce drugs, agrochemicals, or herbicides. The purity of educts is of high importance because impurities in the educt are directly associated with impurities in the product. Because of their high polarity and tendency to form boroxines, boronic acids require derivatization for GC analysis. The presented nano-LC-EI/MS method is easily applicable for a broad range of boronic acids. The method shows good detection limits for boronic acids up to 200 pg, is perfectly linear, and shows a very high robustness and reproducibility. A mixture of compounds could easily be separated on a monolithic RP18e column. The method represents a new, simple, robust, and reproducible approach for the detection of polar analytes. It is a good candidate to become a standard method for industrial applications.
Flender
Cornelia
C
Merck KGaA, Frankfurter Strasse 250, 64293 Darmstadt, Germany. Cornelia.Flender@merck.de
Leonhard
Peter
P
Wolf
Christian
C
Fritzsche
Matthias
M
Karas
Michael
M
D001897:Boronic Acids / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid / Q000379:methods*; D004583:Electrons; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000032:analysis; D012015:Reference Standards
D001897:Boronic Acids; D004364:Pharmaceutical Preparations