Atmospheric Pressure Electrospray Ionization Mass Spectra of Glucose and 2-Fluorodeoxyglucose for Quantitative Analysis of 2-Fluorodeoxyglucose by High-Performance Liquid Chromatography

Abstract

2-Fluoro-2-deoxy-D-glucose (FDG) labeled by fluorine-18 is the most widely used radiopharmaceutical for positron emission tomography (PET). For high-performance liquid chromatography (HPLC)/MS assay and quality control, the mass spectra of FDG and glucose (Glc) in organic + water solutions were studied by flow injection analysis (FIA) and in a chromatographic eluate. In acetonitrile (MeCN) + 0.025% ammonium formate (NH(4)HCO(2)) solvent (80 : 20), electrospray ionisation (ESI) of glucose-FDG provides M.NH(4)(+) and 2M.Na(+) (M = Glc or FDG) as the most intense positive ions. Formation of the latter ions and also of M.MeCN.Na(+) and 2MeCN. Na(+) is typical of the presence of NaCl in the ESI inlet. The positive ions include heavier ions corresponding to the impurities separated by HPLC and also to the cross-ring fragmentation of complexes (2FDG. aMeCNX)L, where a = 0 or 1, L is either Na(+) or NH(4)(+) and X is a fragmented pyranose or anhydropyranose residue. The second most abundant Glc negative ion is m/z = 359 which was interpreted as (2GlcH(+))(). The negative-ion spectrum of FDG has dominating lines due to FDG.HCO(2)() ions at m/z 227 and also (2FDGH(+))() at m/z 363. The m/z 363 signal is suppressed in the presence of NaCl at a molar ratio of 4 : 1 to NH(4)HCO(2), while the ions at m/z 217 and 219, i.e. FDG.Cl(), become three times more intense than FDG.HCO(2)(). The latter ion appears to be most suitable as an analytical signal for chemical analysis of FDG at m/z 226 and 227. Limits of FDG quantitation (LOQ) of 19 ng and 21 ng were found for the 200(+) and 227() ion signals, respectively, and are wholly adequate for verification of total FDG content in radiopharmaceuticals.

Sophorolipid Biosurfactant Can Control Cutaneous Dermatophytosis Caused by Trichophyton mentagrophytes

“…The UPLC-ESI-MS analyses of the sugar components of both the samples confirmed glucose as the sole monomer present, and no other sugars were detected, confirming SL-YS3 to be an SL type of biosurfactant. The mass spectral analyses substantiated the same upon comparison with previous literature (Macášek et al, 2003;Pathak et al, 2015).…”

Simple and Fast Method for Recognition of Reducing and Nonreducing Neutral Carbohydrates by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

“…The lack of acidic sites in neutral oligosaccharides reducing the ability of forming the deprotonated molecules ([M − H] - ) is probably the reason for the small number of the papers dealing with the negative-ion MALDI Time of Flight (TOF) MS analyses of neutral oligosaccharides ( , ). Alternative ways to charge the neutral oligosaccharides are either attachment of a small inorganic anion A - to form the anionic adduct [M + A] - ( , ) or covalent binding of negatively charged labels ( − ). There is no general anion dopant for oligosaccharide analysis by MALDI-TOF MS; by now, mainly hydrogen sulfate and chloride are used ( , ).…”

Quality control of PET radiopharmaceuticals by high‐performance liquid chromatography with tris(2,2′‐bipyridyl)ruthenium(II) electrogenerated chemiluminescence detection

“…Various methods have been described to determine the quantity of PET molecules in pharmaceutical fl uids: HPLC with UV absorbance, electrochemical (Alexoff et al, 1992;Nakao et al, 2006), mass spectrometry (MS) (Hyllbrant et al, 1999;Macasek et al, 2003) and scintillation proximity assay (Beauregard et al, 2007). Among these methods, LC/MS is perhaps the most sensitive and can give reliable results; however, it requires quite expensive equipment and a higher operating cost, and is therefore not suitable for routine analysis in PET facilities.…”