Rapid screening of polysaccharide-based plasma volume expanders dextran and hydroxyethyl starch in human urine by liquid chromatography-tandem mass spectrometry.
The increasing number of samples and target substances in doping control requires continuously improved screening methods, combining high-throughput analysis, simplified sample preparation, robustness and reliability. Hence, a rapid screening procedure based on liquid chromatography-electrospray ionization-tandem mass spectrometry with in-source collision-induced dissociation was developed. The detection of the polysaccharide-based plasma volume expanders dextran and hydroxyethyl starch (HES) in human urine was established without further sample preparation. The in-source fragmentation strategy of the approach represented a valuable tool in the analysis of the polysaccharide-based compounds, allowing the use of tandem mass spectrometry. After direct injection of urine specimens, analytes were chromatographically separated on a monolithic reverse-phase column and detected via multiple reaction monitoring of diagnostic ions at detection limits of 10 microg/mL for HES and 30 microg/mL for dextran. Validation was performed regarding the parameters specificity, linearity, precision (8-18%) and accuracy (77-105%) and the method was applied to the investigation of approximately 400 doping control samples and seven dextran and two hydroxyethyl starch post-administration samples. The approach demonstrated its capability as a rapid screening tool for the detection of dextran and hydroxyethyl starch and represents an alternative to existing screening procedures since time consuming hydrolysis or derivatization steps were omitted.
Guddat
Sven
S
Institute of Biochemistry, German Sport University, Cologne, Germany. s.guddat@biochem.dshs-koeln.de
Thevis
Mario
M
Thomas
Andreas
A
Schänzer
Wilhelm
W
D002853:Chromatography, Liquid / Q000379:methods*; D003911:Dextrans / Q000737:chemistry / Q000652:urine*; D005260:Female; D006801:Humans; D006895:Hydroxyethyl Starch Derivatives / Q000737:chemistry / Q000652:urine*; D008297:Male; D010952:Plasma Substitutes / Q000032:analysis* / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*
D003911:Dextrans; D006895:Hydroxyethyl Starch Derivatives; D010952:Plasma Substitutes