High-performance liquid chromatography/inductively coupled plasma mass spectrometry and tandem mass spectrometry for the detection of carbon-containing compounds.
High-performance liquid chromatography (HPLC) combined with inductively coupled plasma mass spectrometry (ICPMS) has been studied as a means for the detection of carbon to provide a 'universal' method for detecting organic compounds in chromatographic eluents. Carbon is particularly difficult to ionise and the amount of carbon present in normal chromatographic systems leads to high backgrounds, making detection a challenge. Novel separation approaches were therefore employed, using either entirely aqueous eluents (at temperatures of 60 and 160 degrees C, dependent on the column used) to eliminate the organic modifier completely, or isotopically enriched solvents. For the aqueous eluents, detection limits for sulphanilamide were found to be 2.26 microg, corresponding to 1.13 micromol (0.47 micromol of carbon), injected on a conventional 4.6 mm i.d. column. The use of a narrow bore column with highly isotopically enriched 12C-methanol (99.95 atom%) as organic modifier for the mobile phase enabled the detection of 86 micromol for 13C-triple-labelled caffeine and 79 micromol for 13C-double-labelled phenacetin. The sensitive detection of 12C-compounds with 13C-enriched methanol as organic modifier proved impractical due to a lower level of isotopic enrichment (99 atom%) of this solvent, with the residual 12C-methanol resulting in significant interference.
Smith
Christopher
C
Department of Drug Metabolism and Pharmacokinetics, AstraZeneca, Mereside, Alderley Park, Macclesfield SK10 4TG, UK. Christopher.smith1@astrazeneca.com
Jensen
Berit Packert
BP
Wilson
Ian D
ID
Abou-Shakra
Fadi
F
Crowther
David
D
D000983:Antipyrine / Q000032:analysis / Q000737:chemistry; D002110:Caffeine / Q000032:analysis / Q000737:chemistry; D002244:Carbon / Q000032:analysis* / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D010615:Phenacetin / Q000032:analysis / Q000737:chemistry; D012997:Solvents / Q000737:chemistry; D000077145:Sulfanilamide; D013424:Sulfanilamides / Q000032:analysis / Q000737:chemistry
D012997:Solvents; D013424:Sulfanilamides; D000077145:Sulfanilamide; D002110:Caffeine; D002244:Carbon; D010615:Phenacetin; D000983:Antipyrine