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DETERMINATION OF ANDROGENIC STEROIDS IN URINE BY GC-MS Angel Totoricagüena, Silvio D. Barletta and Carlos E. Alli Sector of Active Substances and Chemical Residues, General Direction of Laboratory - National Service of Health and Agri-Food Quality (SENASA) - Argentina Contact: [email protected] - [email protected] - [email protected] Introduction Figure 1. Chemical structures of studied androgens. Methods GC-MS Conditions Talcahuano 1660 CP 1640, Martinez, Buenos Aires, Argentina www.senasa.gob.ar Samples Preparation Results Figure 3. Linearity of MTST and β-BLD with d3-BLD. Figure 4. Linearity of α-NTT and β-NTT with d3-TST. Figure 2. a) Chromatogram of MTST (RT: 20.167 min); b) Chromatogram of β-BLD and d3- BLD (RT: 21.874 min); c) Chromatogram of α-NTT/ β-NTT and d3-TST (RT: 21.795/22.722 and 23.001). All results obtained for the studied parameters, linearity, reproducibility and repeatability, selectivity and ruggednnes are in accordance with SENASA Resolution N°138/2002 and its modifying dispositions Nº 125/200 6 and Nº 06/2004, as well as EU Council Directive 2002/657/EC. This method also demonstrates its effectiveness for the identification and quantification of Methyl Boldenone in urine by GC-MS. Analyte Analytical range (µg/l) Average recovery % LD o CCα (µg/l) CCβ (µg/l) α-NTT 0.96 – 7.97 96.2 0.32 0.55 β-NTT 0.56 – 4.51 95.8 0.12 0.26 β-BLD 0.58 – 4.63 100.4 0.11 0.13 MTST 0.99 – 7.88 99.5 0.19 0.34 Conclusions Table 1. Validation parameters obtained for each androgenic steroid.
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Page 1: DETERMINATION OF ANDROGENIC STEROIDS IN URINE ... 202.pdfPOSTER ANDROGENICOS 2-FINAL - A4 Author calli Created Date 5/23/2016 9:40:19 AM ...

DETERMINATION OF ANDROGENIC STEROIDS IN URINE BY GC-MS

Angel Totoricagüena, Silvio D. Barletta and Carlos E. Alli

Sector of Active Substances and Chemical Residues, General Direction of Laboratory - National Service of Health and Agri-Food Quality (SENASA) - ArgentinaContact: [email protected] - [email protected] - [email protected]

Introduction

Figure 1. Chemical structures of studied androgens.

Methods

GC-MS Conditions

Talcahuano 1660CP 1640, Martinez, Buenos Aires, Argentina

www.senasa.gob.ar

Samples Preparation

Results

Figure 3. Linearity of MTST and β-BLD with d3-BLD.

Figure 4. Linearity of α-NTT and β-NTT with d3-TST.Figure 2. a) Chromatogram of MTST (RT: 20.167 min); b) Chromatogram of β-BLD and d3-BLD (RT: 21.874 min); c) Chromatogram of α-NTT/ β-NTT and d3-TST (RT: 21.795/22.722 and 23.001).

All results obtained for the studied parameters, linearity, reproducibility and repeatability, selectivity and ruggednnes are in accordance with SENASA Resolution N°138/2002 and its modifying dispositions Nº 125/200 6 and Nº 06/2004, as well as EU Council Directive 2002/657/EC.This method also demonstrates its effectiveness for the identification and quantification of Methyl Boldenone in urine by GC-MS.

Analyte Analytical range

(µg/l)

Average

recovery %

LD o CCα

(µg/l)

CCβ

(µg/l)

α-NTT 0.96 – 7.97 96.2 0.32 0.55

β-NTT 0.56 – 4.51 95.8 0.12 0.26

β-BLD 0.58 – 4.63 100.4 0.11 0.13

MTST 0.99 – 7.88 99.5 0.19 0.34

Conclusions

Table 1. Validation parameters obtained for each androgenic steroid.

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