TY - JOUR
T1 - Determination of anabolic agents in dietary supplements by liquid chromatography-high-resolution mass spectrometry
AU - Odoardi, Sara
AU - Castrignanò, Erika
AU - Martello, Simona
AU - Chiarotti, Marcello
AU - Strano-Rossi, Sabina
N1 - Funding Information:
This work was performed under the framework of the project ‘Smart-Stop’, funded by the Italian Antidrug Policies Department
Publisher Copyright:
© 2015, © 2015 Taylor & Francis.
PY - 2015/5/4
Y1 - 2015/5/4
N2 - A sensitive method for the identification and quantification of anabolic steroids and clenbuterol at trace levels in dietary supplements by liquid chromatography-high-resolution mass spectrometry (LC-HRMS) in atmospheric pressure ionisation (APCI) mode using a single-stage Orbitrap analyser operating at a resolution power of 100 000 full width at half maximum (FWHM) was developed and validated. A total of 1 g of dietary supplement was added with testosterone-d3 as internal standard, dissolved in methanol, evaporated to dryness, diluted in sodium hydroxide solution and extracted with a mixture of pentane/ethyl ether 9:1. The extract was directly injected into the LC-HRMS system. The method was fully validated. Limits of detection (LODs) obtained for anabolic androgenic steroids (AASs) varied from 1 to 25 ng g−1 and the limit of quantitation (LOQ) was 50 ng g−1 for all analytes. The calibration was linear for all compounds in the range from the LOQ to 2000 ng g−1, with correlation coefficients always higher than 0.99. Accuracy (intended as %E) and repeatability (%CV) were always lower than 15%. Good values of matrix effect and recovery were achieved. The ease of the sample preparation together with a fast run time of only 16 min permitted rapid identification of the analytes. The method was applied to the analysis of 30 dietary supplements in order to check for the presence of anabolic agents not labelled as being present in these supplements. Many AASs were often detected in the same sample: indeed, androstenedione was detected in nine supplements, 5-androsten-3β-ol-17-one (DHEA) in 12, methandienone in three, stanozolol in one, testosterone in seven and testosterone esters in four of them. A retrospective analysis of suspected compounds not included at the beginning of the method development was also possible by means of the full acquisition spectra obtained with the HRMS technique.
AB - A sensitive method for the identification and quantification of anabolic steroids and clenbuterol at trace levels in dietary supplements by liquid chromatography-high-resolution mass spectrometry (LC-HRMS) in atmospheric pressure ionisation (APCI) mode using a single-stage Orbitrap analyser operating at a resolution power of 100 000 full width at half maximum (FWHM) was developed and validated. A total of 1 g of dietary supplement was added with testosterone-d3 as internal standard, dissolved in methanol, evaporated to dryness, diluted in sodium hydroxide solution and extracted with a mixture of pentane/ethyl ether 9:1. The extract was directly injected into the LC-HRMS system. The method was fully validated. Limits of detection (LODs) obtained for anabolic androgenic steroids (AASs) varied from 1 to 25 ng g−1 and the limit of quantitation (LOQ) was 50 ng g−1 for all analytes. The calibration was linear for all compounds in the range from the LOQ to 2000 ng g−1, with correlation coefficients always higher than 0.99. Accuracy (intended as %E) and repeatability (%CV) were always lower than 15%. Good values of matrix effect and recovery were achieved. The ease of the sample preparation together with a fast run time of only 16 min permitted rapid identification of the analytes. The method was applied to the analysis of 30 dietary supplements in order to check for the presence of anabolic agents not labelled as being present in these supplements. Many AASs were often detected in the same sample: indeed, androstenedione was detected in nine supplements, 5-androsten-3β-ol-17-one (DHEA) in 12, methandienone in three, stanozolol in one, testosterone in seven and testosterone esters in four of them. A retrospective analysis of suspected compounds not included at the beginning of the method development was also possible by means of the full acquisition spectra obtained with the HRMS technique.
KW - anabolic agents
KW - dietary supplements analysis
KW - drug testing
KW - LC-HRMS
UR - http://www.scopus.com/inward/record.url?scp=84926193573&partnerID=8YFLogxK
U2 - 10.1080/19440049.2015.1014868
DO - 10.1080/19440049.2015.1014868
M3 - Article
C2 - 25719897
AN - SCOPUS:84926193573
SN - 1944-0049
VL - 32
SP - 635
EP - 647
JO - Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment
JF - Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment
IS - 5
ER -
