TY - JOUR
T1 - LC/MS quantitative study of glucose by iodine attachment
AU - Rogatsky, Eduard
AU - Tomuta, Vlad
AU - Stein, Daniel T.
N1 - Funding Information:
This research was supported by grants from the American Diabetes Association, NIH/NCRR and NIDDK: MO1-RR12248 (GCRC) and R01 DK61644-01.
PY - 2007/5/22
Y1 - 2007/5/22
N2 - We explored the potential of iodine attachment to improve the sensitivity of glucose measurement by LC/MS. After sample preparation, glucose was separated by normal phase chromatography, followed by anionization by I--attachment prior to MS by post-column addition of a methanolic solution of iodoform. Iodine is capable of forming an anionic adduct with neutral monosaccharides in negative ion mode electrospray mass spectrometry. Quasi-molecular ions [M + I]- of glucose, and [6,6-2H2]glucose (abbreviated d2-glucose) internal standard were quantitated in selected ion monitoring (SIM) mode. Iodine attachment LC/MS analysis provided high sensitivity, superior to GC/MS. It greatly simplified sample preparation and increased throughput. The advantages of iodine attachment can be realized even on old mass spectrometers. A LOD of 50 pg glucose on column was achieved. Due to iodine's predisposition to sublimate, the iodoform concentration must be minimized, which adds complexity to method development. To optimize reagent concentration we developed an efficient and flexible gradient-based delivery platform. Strategy for method development with iodoform is given.
AB - We explored the potential of iodine attachment to improve the sensitivity of glucose measurement by LC/MS. After sample preparation, glucose was separated by normal phase chromatography, followed by anionization by I--attachment prior to MS by post-column addition of a methanolic solution of iodoform. Iodine is capable of forming an anionic adduct with neutral monosaccharides in negative ion mode electrospray mass spectrometry. Quasi-molecular ions [M + I]- of glucose, and [6,6-2H2]glucose (abbreviated d2-glucose) internal standard were quantitated in selected ion monitoring (SIM) mode. Iodine attachment LC/MS analysis provided high sensitivity, superior to GC/MS. It greatly simplified sample preparation and increased throughput. The advantages of iodine attachment can be realized even on old mass spectrometers. A LOD of 50 pg glucose on column was achieved. Due to iodine's predisposition to sublimate, the iodoform concentration must be minimized, which adds complexity to method development. To optimize reagent concentration we developed an efficient and flexible gradient-based delivery platform. Strategy for method development with iodoform is given.
KW - Glucose
KW - Human plasma
KW - Iodine attachment
KW - Isotope dilution assay
KW - Liquid chromatography-mass spectrometry
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U2 - 10.1016/j.aca.2007.04.001
DO - 10.1016/j.aca.2007.04.001
M3 - Article
C2 - 17481402
AN - SCOPUS:34247483053
SN - 0003-2670
VL - 591
SP - 155
EP - 160
JO - Analytica Chimica Acta
JF - Analytica Chimica Acta
IS - 2
ER -