The accurate determination of serum glucose by isotope dilution mass spectrometry—two methods

Abstract

Two isotope dilution mass spectrometric methods have been developed for the determination of D-glucose in human serum. Each uses a uniformly labeled (13C)glucose as the internal standard. The first method involves conversion of glucose into 1,2:5,6-di-O-isopropylidene-alpha-D-glucofuranose and an extensive clean-up, followed by quantitation using packed column gas chromatography mass spectrometry. In the second method, glucose is converted into alpha-D-glucofuranose cyclic 1,2:3,5-bis(butylboronate)-6-acetate. The wet chemistry work-up is simpler, but analysis by capillary gas chromatography mass spectrometry is required. Both methods exhibit excellent precision (coefficients of variation less than 0.3%) and provided mean values that agree within 1% for all serum pools tested.

High‐precision mass spectrometric analysis using stable isotopes in studies of children

“…The various methods to determine plasma glucose enrichments involve different cleanup and derivatization techniques, such as trimethylsilyl (Bjorkhem et al, 1976;Bier et al, 1977;Jansen et al, 1986;Kury & Keller, 1991;Rojas-Escudero et al, 2004), pentaacetate (van Dijk et al, 2003;van der Schoor et al, 2004), butyl boronic acid (White et al, 1982;Pickert et al, 1991;Clapperton, Coward, & Bluck, 2002) and aldonitrile pentaacetate (Tserng & Kalhan, 1983;Magni et al, 1992) derivatization in combination with GC/MS measurements in the electron impact (EI) (Desage et al, 1989) or chemical ionization (CI) mode (Tayek, Bergner, & Lee, 1991;Guo et al, 1992).…”

NIST's Role in Measurement Accuracy for Diagnosis and Monitoring of Diabetes

“…The definitive method that NIST uses is described elsewhere in detail. 3 The method involves adding to a known mass of serum a known quantity of an internal standard in the form of glucose with six 13 C replacing the predominant 12 C found in natural glucose. After allowing the added labeled form and the native form to equilibrate, the sample is treated with ethanol to precipitate protein and is put through a mixed resin ion exchange column to remove nonvolatile ionic species.…”

Developing a reference measurement procedure for free glycerol in human serum by two-step gas chromatography–isotope dilution mass spectrometry

“…Isotope dilution mass spectrometry (IDMS) is recognized to be a primary method [16][17][18], which has been widely used to establish reference measurement procedures for organic biomarkers such as creatinine [19][20][21], glucose [22][23][24], cholesterol [25][26][27], urea [28,29], uric acid [30,31] and triglycerides [32,33]. A GC-IDMS method for free glycerol measurement was reported previously [13].…”