TY - JOUR
T1 - Determination of prohibited, small peptides in urine for sports drug testing by means of nano-liquid chromatography/benchtop quadrupole orbitrap tandem-mass spectrometry
AU - Thomas, Andreas
AU - Walpurgis, Katja
AU - Krug, Oliver
AU - Schänzer, Wilhelm
AU - Thevis, Mario
N1 - Copyright © 2012 Elsevier B.V. All rights reserved.
PY - 2012/10/12
Y1 - 2012/10/12
N2 - In the present study, a screening assay was developed comprising 11 prohibited peptides (<1.5 kDa) that are sufficiently purified from urine using weak cation exchange with subsequent determination of all substances by means of nanoUHPLC separation coupled to high resolution tandem mass spectrometry. These peptides included Gonadorelin (LH-RH), Desmopressin and 9 growth hormone releasing peptides (GHRP-1, -2, -4, -5, -6, Hexarelin, Alexamorelin, Ipamorelin and a GHRP-2 metabolite); however, the procedure is expandable to further target analytes or metabolites. The method was validated with a main focus on qualitative result interpretation considering the parameters specificity, linearity (0-500 pg/mL), recovery (45-95%), precision (<20% at 100 pg/mL), limits of detection (2-10 pg/mL), robustnesss and ion suppression. The proof-of-principle was shown by analysing excretion study urine samples for LHRH, Desmopressin and GHRP-2.
AB - In the present study, a screening assay was developed comprising 11 prohibited peptides (<1.5 kDa) that are sufficiently purified from urine using weak cation exchange with subsequent determination of all substances by means of nanoUHPLC separation coupled to high resolution tandem mass spectrometry. These peptides included Gonadorelin (LH-RH), Desmopressin and 9 growth hormone releasing peptides (GHRP-1, -2, -4, -5, -6, Hexarelin, Alexamorelin, Ipamorelin and a GHRP-2 metabolite); however, the procedure is expandable to further target analytes or metabolites. The method was validated with a main focus on qualitative result interpretation considering the parameters specificity, linearity (0-500 pg/mL), recovery (45-95%), precision (<20% at 100 pg/mL), limits of detection (2-10 pg/mL), robustnesss and ion suppression. The proof-of-principle was shown by analysing excretion study urine samples for LHRH, Desmopressin and GHRP-2.
KW - Chromatography, Liquid
KW - Doping in Sports
KW - Female
KW - Humans
KW - Limit of Detection
KW - Linear Models
KW - Male
KW - Nanotechnology
KW - Oligopeptides
KW - Reproducibility of Results
KW - Substance Abuse Detection
KW - Tandem Mass Spectrometry
U2 - 10.1016/j.chroma.2012.07.022
DO - 10.1016/j.chroma.2012.07.022
M3 - Journal articles
C2 - 22901302
SN - 1873-3778
SN - 0021-9673
VL - 1259
SP - 251
EP - 257
JO - Journal of chromatography. A
JF - Journal of chromatography. A
ER -