TY - JOUR
T1 - Screening for exogenous androgen anabolic steroids in human hair by liquid chromatography/orbitrap-high resolution mass spectrometry
AU - Strano-Rossi, Sabina
AU - Castrignanò, Erika
AU - Anzillotti, Luca
AU - Odoardi, Sara
AU - De-Giorgio, Fabio
AU - Bermejo, Ana
AU - Pascali, Vincenzo L.
N1 - Funding Information:
The authors acknowledge Italian Ministry of Research for financing this study, that was developed in part in the framework of FIRB project code RBFR12LD0W_002. We are also grateful to Thermo Fisher Scientific, in particular to Igor Fochi for his invaluable technical help in the phases of instrumental setup and method development.
PY - 2013/9/2
Y1 - 2013/9/2
N2 - A method for the screening of various anabolic steroids and their esters in human hair, based on liquid-chromatography-high resolution mass spectrometry using an Exactive benchtop Orbitrap mass spectrometer, has been set up and validated. This method involved methanolic incubation of 30. mg of hair and analysis of the relevant extract in HPLC using a C18 column. The mass detector, with nominal resolving power of 100,000, operated in full scan mode in APCI under positive ionization mode. Analytes were identified by exact mass, correspondence of isotopic cluster and retention times.The limits of detection obtained varied from 10 to 50pgmg-1, and limits of quantitation were 0.5ngmg-1 for all compounds. The method was linear for all analytes in the ranges from the LOQ to 6ngmg-1, giving correlation coefficients >0.99 for all analytes. Also accuracy (intended as %E) and repeatability (%CV) were always lower than 15%. Specificity was assessed by analysing ten blank samples and fifteen samples from polidrug abusers. This method was applied to a real-life case, resulting in the identification of testosterone undecanoate in the hair of a suspect. The analyte identity was confirmed by the analysis of its in-source fragmentation and comparison to a certified standard. Thanks to the scan acquisition, this method also enables retrospective re-analysis of the acquired datafile in case a further analyte needs to be screened.
AB - A method for the screening of various anabolic steroids and their esters in human hair, based on liquid-chromatography-high resolution mass spectrometry using an Exactive benchtop Orbitrap mass spectrometer, has been set up and validated. This method involved methanolic incubation of 30. mg of hair and analysis of the relevant extract in HPLC using a C18 column. The mass detector, with nominal resolving power of 100,000, operated in full scan mode in APCI under positive ionization mode. Analytes were identified by exact mass, correspondence of isotopic cluster and retention times.The limits of detection obtained varied from 10 to 50pgmg-1, and limits of quantitation were 0.5ngmg-1 for all compounds. The method was linear for all analytes in the ranges from the LOQ to 6ngmg-1, giving correlation coefficients >0.99 for all analytes. Also accuracy (intended as %E) and repeatability (%CV) were always lower than 15%. Specificity was assessed by analysing ten blank samples and fifteen samples from polidrug abusers. This method was applied to a real-life case, resulting in the identification of testosterone undecanoate in the hair of a suspect. The analyte identity was confirmed by the analysis of its in-source fragmentation and comparison to a certified standard. Thanks to the scan acquisition, this method also enables retrospective re-analysis of the acquired datafile in case a further analyte needs to be screened.
KW - Anabolic steroids
KW - Esters
KW - Forensic toxicology
KW - Hair analysis
KW - High resolution mass spectrometry
KW - Orbitrap
UR - http://www.scopus.com/inward/record.url?scp=84881611215&partnerID=8YFLogxK
U2 - 10.1016/j.aca.2013.07.028
DO - 10.1016/j.aca.2013.07.028
M3 - Article
C2 - 23953207
AN - SCOPUS:84881611215
SN - 0003-2670
VL - 793
SP - 61
EP - 71
JO - ANALYTICA CHIMICA ACTA
JF - ANALYTICA CHIMICA ACTA
ER -