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Quantitative analysis of the molecular species of monosialogangliosides by continuous‐flow fast‐atom bombardment mass spectrometry
Author(s) -
Chen S.,
Pieraccini G.,
Moneti G.
Publication year - 1991
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.1290051210
Subject(s) - chemistry , mass spectrometry , chromatography , fast atom bombardment , analytical chemistry (journal) , detection limit , quantitative analysis (chemistry) , calibration curve , deprotonation , standard curve , ion , organic chemistry
Negative‐ion continuous‐flow fast‐atom bombardment mass spectroemtry was evaluated asa means for the quantitative analysis of N ‐acetylneuraminyl‐galactosyl‐glucosyl ceramide (NeuAc‐G M 3) and N ‐acetylgalactosaminyl‐( N ‐acetylneuraminyl)galactosyl‐glucosyl‐ceramide (NeuAc‐G M 3). This study was carried out on a 7070‐EQ mass spectrometer (VG Analytical, Manchester, UK) using a home‐made continuous‐flow fast‐atom bombardment probe with a mixture of methanol +water+triethanolamine (70:27:3, v/v/v)as the mobile phase. Utilizing 100 ng of acetyl‐lysogalactosyl‐ N ‐acetylgalactosaminyl‐( N ‐acetylneuraminyl)galactosyl‐glucosylceramide (acetyl‐lysoG M 1) as an internal standard curves for NeuAc‐G M3 d18:1‐16 0, NeuAc‐G M 3d18:1‐18:0 and Neuac‐G M 3d18:1‐18:0 were found to be linear over the range 5‐250ng, with associated correlation coefficients of 0.990‐0.997. The lower limit of detection was found to be 2.5ng. Satisfactory results could also de obtained when the calibration curves were derived from the deprotonated molecular ions of a mixture of the NeuAc‐ M 2and NeuAc‐G M 3classes. Using this approach, quantitative determination of NeuAc‐G M 3d18:1‐16:0 from rat adrenal gland was performed sing N ‐acetylneuraminic acid assay as a test control. We found 278±36 ng of this species in 1 mg of tissue (three replicate experiments). The procedure represents a senstive method for the quantitation of mionosialogangliosides and its capability to give molecular species information.