Rapid analysis of anabolic steroid metabolites in urine by combining field asymmetric waveform ion mobility spectrometry with liquid chromatography and mass spectrometry

TY - JOUR

T1 - Rapid analysis of anabolic steroid metabolites in urine by combining field asymmetric waveform ion mobility spectrometry with liquid chromatography and mass spectrometry

AU - Arthur, Kayleigh L.

AU - Turner, Matthew A.

AU - Brailsford, Alan D.

AU - Kicman, Andrew T.

AU - Cowan, David A.

AU - Reynolds, James C.

AU - Creaser, Colin S.

PY - 2017/7/18

Y1 - 2017/7/18

N2 - The combination of field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry (LC-FAIMS-MS) has been developed for the analysis of glucuronide and sulfate metabolites of seven anabolic-androgenic steroids AAS in urine. Separation by FAIMS-MS was investigated in positive ion mode for selected cationic adducts (H+, NH4+, Na+, K+, Cs+). LC-FAIMS-MS analysis of the doubly sodiated adducts ([M+2Na-H]+) of isobaric and co-eluting steroid metabolites allowed their rapid (8 min) qualitative and quantitative determination in spiked urine using hydrophilic interaction liquid chromatography prior to FAIMS-MS separation, with discrimination >95% achieved between the steroids investigated. A quantitative evaluation of the LC-FAIMS-MS method was performed giving limits of detection in the range 1-6 ng mL-1, limits of quantification in the range 3-20 ng mL-1, with reproducibility (%RSD <10%; n=6) and linearity (R2> 0.99). The LC-FAIMS-MS method demonstrates increases in signal-to-noise ratios for the doubly sodiated steroid metabolites in unspiked urine (>250%) by the reduction of isobaric interferences from the matrix. An alternative or additional tool for identification of the steroid metabolites is based on the observations of different patterns of sodium acetate clusters that are characteristic for each metabolite.

AB - The combination of field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry (LC-FAIMS-MS) has been developed for the analysis of glucuronide and sulfate metabolites of seven anabolic-androgenic steroids AAS in urine. Separation by FAIMS-MS was investigated in positive ion mode for selected cationic adducts (H+, NH4+, Na+, K+, Cs+). LC-FAIMS-MS analysis of the doubly sodiated adducts ([M+2Na-H]+) of isobaric and co-eluting steroid metabolites allowed their rapid (8 min) qualitative and quantitative determination in spiked urine using hydrophilic interaction liquid chromatography prior to FAIMS-MS separation, with discrimination >95% achieved between the steroids investigated. A quantitative evaluation of the LC-FAIMS-MS method was performed giving limits of detection in the range 1-6 ng mL-1, limits of quantification in the range 3-20 ng mL-1, with reproducibility (%RSD <10%; n=6) and linearity (R2> 0.99). The LC-FAIMS-MS method demonstrates increases in signal-to-noise ratios for the doubly sodiated steroid metabolites in unspiked urine (>250%) by the reduction of isobaric interferences from the matrix. An alternative or additional tool for identification of the steroid metabolites is based on the observations of different patterns of sodium acetate clusters that are characteristic for each metabolite.

KW - Journal Article

UR - http://www.scopus.com/inward/record.url?scp=85025701259&partnerID=8YFLogxK

U2 - 10.1021/acs.analchem.7b00940

DO - 10.1021/acs.analchem.7b00940

M3 - Article

C2 - 28613840

SN - 0003-2700

VL - 89

SP - 7431

EP - 7437

JO - Analytical Chemistry

JF - Analytical Chemistry

IS - 14

ER -