Open AccessDEVELOPMENT OF A TECHNIQUE FOR THE MASS-SPECTROMETRIC DETERMINATION OF GONADOTROPIN-RELEASING HORMONE AND ITS ANALOGS FOR DOPING CONTROL
Author(s) -
Ksenia Shestakova,
Grigory Dudko,
М. А. Дикунец
Publication year - 2017
Publication title -
tonkie himičeskie tehnologii
Language(s) - English
Resource type - Journals
eISSN - 2686-7575
pISSN - 2410-6593
DOI - 10.32362/2410-6593-2017-12-2-81-99
Subject(s) - chromatography , analyte , ion suppression in liquid chromatography–mass spectrometry , chemistry , detection limit , electrospray , selected reaction monitoring , solid phase extraction , tandem mass spectrometry , high performance liquid chromatography , mass spectrometry , extraction (chemistry) , matrix (chemical analysis) , liquid chromatography–mass spectrometry , analytical chemistry (journal)
In the present study, a rapid, sensitive, and selective method for determination of several synthetic analogues of gonadotropin-releasing hormone in human urine by solid-phase extraction and ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed. Various parameters affecting sample preparation, LC separation, and MS/MS detection were investigated, and optimized conditions were identified. The UPLC-MS/MS system was equipped with an electrospray ion source operating in positive ion mode with selected reaction monitoring. Leuprolide-13С6 was used as internal standard for analytes quantitative assessment. The proposed method was validated considering the parameters specificity, linearity (0.1-10 ng/ml), recovery (52-98%), limit of detection (0.1 ng/ml), matrix effects and stability.