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Quantitative determination of glucose in serum by isotope dilution mass spectrometry following gas liquid chromatography with fused silica column
Author(s) -
Pelletier Omer,
Cadieux Serge
Publication year - 1983
Publication title -
biomedical mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 0306-042X
DOI - 10.1002/bms.1200100306
Subject(s) - chromatography , chemistry , mass spectrometry , isotope dilution , derivatization , gas chromatography , monosaccharide , gas chromatography–mass spectrometry , selected ion monitoring , analytical chemistry (journal) , biochemistry
Abstract To evaluate the accuracy of glucose methods, we have set up an isotope dilution gas chromatographic mass spectrometric method where methyloxime trimethylsilyl derivatives of monosaccharides were separated with a SP‐2100 fused silica column. An autodiluter was found suitable for delivering aliquots for derivatization: CV of 0.13% (aqueous) and 0.24% (serum). Ions at m / z 319 (non‐labelled) and 323 (deuterium‐labelled) were selected for glucose, galactose and mannose, and at m / z 307 and 311 for fructose. Optimization of ion monitoring with a Finnigan 4000 gas chromatograph mass spectrometer 6110 data system was limited to one scan per second without full compensation for 0.1 u shifts. A CV of 0.65% in isotope ratios was obtained for 30 injections (three per vial) of one glucose standard. A similar variation between duplicate injections was obtained with serum. Glucose measurements on 36 serum specimens (six individuals) were made by gas chromatography mass spectrometry and by both a manual (reference) and a flow‐through method using hexokinase and glucose‐6‐phosphate dehydrogenase. Mean glucose by gas chromatography mass spectrometry was 5.57 mmol l −1 ; bias was −1.7% manually and +1.2% by the automated method. Average concentrations (mmol l −1 ) of other hexoses were low: mannose (0.058), fructose (0.015) and galactose (0.005). Glucose measurements of two control sera bracketed with standards showed satisfactory agreeement between the three methods. CV of 1.2 to 1.4% by gas chromatography mass spectrometry indicate that further refinements are required.