-\ L. I u r b I ! U rJ, L. U (1 Response Ratio 3- 2.5- 2- 1.5- 1- . 0.5- testosterone Resp Ratio = 8.95e-001 * Amt Coef of Det (r*2} = 0.992 Curve Fit: Linear/(0,0) Method Name : D : \MSDCHEM\ 1\METH0DS\MAN2 7 . M Calibration Table Last Updated: Mon Jul 24 17:15:46 2006 USADA 0088 "^^i ;i rJ r A i I f1 u u [J IJ Response Ratio epitestosterone 0.5- 0.4- 0.3- 0.2- 0.1- 0.2 0.4 Amount Ratio 0.6 Resp Ratio = 9.23e-001 * Arat Coef of Det (r*2) = 0.993 Curve Fit: Linear/(0,0} Method Name: D:\MSDCHEM\l\METHODS\MaN27.M Calibration Table Last Updated: Mon Jul 24 17:15:46 2006 USADA 0089 ^o J. !i File: D:\Msd2 0\juil0 6\24 07\BLUlTE.D Operator: 28 Date Acquired: 24 Jul 2006 12:57 Instrument: MSD 20 Method Pile: MAN2 7 Sample Name : blu te Misc Info: Vial Number : 3 L! I L r'j I Analyse quantitative : Testosterone/Epi testosterone Xbundance 400000 3DO0O0 200000 100000 TIC:BLU1TE,D rim6-> 5.00 > ' :'■, '; v.-i 10.00 15.00 20.00 J SI :METHYLTESTOSTEROHE ^b«Jndance \vx 301 ,30 (301 .00 to 30200): BLU1TE D '.93 120000 100000 eoooo 60000 40000 20000 rime— > 1 21, 46 I , I r r ^ I' r-i- i , •^ff i i 20.50 21.00 21,50 22.00 22.50 r^ Epitestosterone-Testosterone Abundance 3500 Ion 432,40 (432,10 to433,10): BLUITED t 3000 2500 18,41 2000 1500 1000 500 n r\J. 18,97 j\ M-S3 20.26 J rime-> 18,50 19,00 19,50 20,00 20.50 ' 1 ; Epltesto-Testo-llbetaOH A et E Uiundance 3500 Ion 432,40 (432.10 to 433,1 0): BLU1TE,D Ion 522,50 (522.20 to 5Z320): BLU1TE.D Z^ 3000 2500 18.41 2000 1500 1000 500 rin»-> ^^ ^_yzKj^r?^^ul ' ' ' 1 ■ ■ ' 1 1 ■ ' 1 ■ 1 ■ ■ ' 1 1 1 1 1 1 1 1 ■ 1 1 1 16,50 19,00 19,50 20,00 20.50 u page 1 USADA 0090 «tL File: D:\Msd20\juil06\2407\BLURlTE.D Operator: 28 Date Acquired: 24 Jul 2006 14:30 Instrument: HSD 2 Method File: MAN27 Sample Name: blute Misc Info: Vial Number : 5 r^ L.I Analyse quantitative :Testosterone/Epi testosterone ri r*; I 1 r L Xbundance TICiBLURITE.D 500000 400000 300000 200000 lOOOOO \ U-*_ii_>- 1^ 1. ..,,..,1 > . 1,. -^ J .^ Up rime-s 5.0 D 10,00 15,00 20.00 SI :METHYLTESTOSTERONE \bunct^nce 150000 10000O 50000 Ion 301 ,30 (301 ,00 ^^ 302.00): BLUR1TE.D 2(194 ),05 20,37 V^1g^^2£TB8?,aSE25Ba3ffigl8£ nrrw-^ 20,50 21.00 21.50 22,00 22,50 L.,i [1 I I u Epitestosterone-Testosterone M»jr>dance 60OO Ion 432,40 (432,10 to 4Ti.10): BLURITE.D 5000 4000 3000 18.41 19,38 1 2000 19.67 20 68 1000 n 18,97 / UbsfU I < I I I I . I I { I < I 1 1 1 . . I 1 1 1 I . 1 . 1 1 1 1 rime-J 1 8.50 1 9,00 1 9,50 20,00 20,50 Epitesto-Testo-llbetaOH A et E Abundance 6000 5000 Ion 432.40 (432,10 to 433,10); BLURITE.D Ion 522,50 (522.20 to 523,20): BLUR1TE,D rirne-> 16.50 19,00 19.50 20,00 20,50 u U page 1 USADA 0091 ^ /■■'-. I , D:\MSO20UUIL06\2407MT«>74T4.D [J Pi ! i Data File Path Data File Name Operator Date Acquired Acq. Method File Sample Name Vial Number Calibration Title Last Calibration Update # Peak Type 1) *ISTD 2) 3) Ret Time 20.96 18.56 19.36 D:\MSD20\JUIL06\2407\ 178D7474.D 28 7/24/2006 13:28 MAN27 178/07 995474 te 4 Quantification T/E (3 points) MonJui 24 17:1 5:46 2006 Signal Name Target Response Amount Units 301.3 17methylteslost6ron€ 6399496 100,00 ng/ml 432.4 epitestosterone 307234 5.20 ng/ml 432.4 testosterone 3513238 61.37 ng/ml ri L; Caicul du rapport T/E Surface Concentration 11.4 11^ !'i r I n u [} J Page 1 o( 1 D:\IVISDchem\Custrpt\MAN27.CRT 7/24/2006 5:17 PM USADA 0092 §3 (■■-' J 1 ■ i i n L' n D File: D:\Msd20\juil06\2407\l7807474.D Operator; 28 Date Acquired: 24 Jul 2006 13:28 Instrument: MSD 20 Method File: MAN27 Sample Name: 178/07 995474 te Miec Info: Vial Number : 4 Analyse quantitative :Testosterone/Epitestosterone r I I i r, t ' r: L L.j n ^bu^da^ce 3000DOO TIC:17807474.D 2500000 2000000 1500000 1000000 500000 rime-> 5. J 1 lUuLi X. jAi_™jJiiu. JjUwJlj M 10.00 15.00 20.00 SI :METHYLTESTOSTERONE "yjundance ion 301 .30 poi.OO to 302.00): 17807474.0 2l96 150000 1 100000 50000 20-48 21.21 22.56 W}Jh.^i\ iiggi5_3^^,fe3i fef rime-^ 20.50 21.00 21.50 22.00 2250 Epitestosterone- Testosterone Sundance 100000 Ion 432.40 (432.10 IS to433.10}:17B07474.D 36 80000 60000 40000 20.05 19.59 A 1 20000 nme-> e.os fi 18.56 \jm\^iM ' 1 ' ' 1 ' 1 1 ' 1 ' 1 ' ' 1 ' ' 1 ' 1 1 1 1 ' 1 18.50 19.00 19.50 20.00 20.50 Epitesto-Testo-llbetaOH A et E Uiundance 120000 100000 80000 60000 40000 20000 Ion 432.40 (432.1Dto433.10); 17807474.D Ion 522,50 (522.20 tOlSpEO): 17807474.0 19.36 Oi=!^ nme-> 16.50 19.00 19.50 20.00 20.50 u page 1 USADA 0093 8k ■ I File: D:\Msd20\juil06\2407\REFlTE.D Operator: 28 Date Acquired: 24 Jul 2006 15:01 Instrument: MSD 2 Method File: MAN27 Sample Name; blu t30 e5 Misc Info: Vial Number : 6 Analyse quantitative :Testosterone/Spitestosterone I I l: r". L. r: I ! L I "i SI :METHYLTESTOSTERONE r LJ Abundance TIC; REF1TE.D 500000 400000 300000 200000 10O0O0 . 1, -j,.aU ,.0-^^ , 1... ^A. ,J Of nme-> 5.0 10.00 15,00 . 1 1 1 20.00 V r 50000 rime-> 20.50 21,00 21.50 22.00 22.50 Epi testosterone -Testosterone Sundance 40000 30000 20000 10000 nme-> Ion 432.40 (432.10 to 433,10): REF1TE.D 1£t32 18-53 184 18.97 \ 1?;?6.8S0,12KBa72O,66 A 18,50 19.00 19.50 20,00 20,50 Epitesto-Testo-llbetaOH A et E yjundance 4000D 30000 20000 10000 rime-> Inn 432,40 (432,10 to 433.10): REF1TE,D ton 522,50 (SSadBKi 523,20): REF1TE.D 18,53 M\ 18-9Ce,1B,}t3 ■'9;^,S20,1ffi{BB720.66 A 16.50 19,00 19,50 20.00 20.50 page 1 USADA 0094 S5 n n File: D:\Msd20\juil06\2407\REF2TE.D Operator: 2 8 Date Acquired: 24 Jul 2006 15:32 Instrument: MSD 20 MAN27 blu tl80 e30 Method File: Sampl e Name : Misc Info: Vial Number 7 n LI Analyse quantitative : Testosterone/Epitestosterone ri r": r\ a Abundance 500000 400000 300000 200000 100000 0^ TIC: REF2TE.D __J_ LLi rime-> 5.00 10.00 15.00 20.00 J SI iMETHYLTESTOSTERONE ^bundance 140000 Ion 301 ,30 (301.00 to 302,00): REF2TE.D ^94 120000 100000 eoooo 60000 40000 20000 rini6-> 20.35 L "^'^ 1 1 ■! y 'I' 1' ^ 1^ 1 1 t 1 P"] T- 1 1 1 1 1 1 r 1 1 1 i^rT= 20.50 21.00 21.50 22.00 22-50 a Epitestosterone-Testosterone Abundance 200000 150000 100000 50000 rime-> Ion 432.40 (432.10 to 433.10): REF2TE.D 1EL32 18.53 1B.4i 19,98 19.EIB.85 2EI:EIB6 I ' ' I ' I ' I ' I I ' ' I I I I ' I I I ' ' I ' I 18.50 19.00 19.50 20.00 20,50 Epitesto-Testo-llbetaOH A et E Abundance 200000 150000 100000 50000 nme-> Ion 432.40 (432.10to 433.10): R6F2TE.D Ion 522.50 {522*32) 523.20): REF2TE,D 18.53 18- OW-r-T-? 13.98 19.eB.B5 2ECE06 I'll I'T'-r-r'T I . I < . I I I I < I 1 r I I I 18.50 19.00 19,50 20,00 20,50 U- page 1 USADA 0095 % =14 . i i.i n File: D:\Msd2 0\juil06\2407\REF3TE.D Operator: 28 Date Acquired: 24 Jul 2006 16:02 Instrument: MSD 20 Method File: MAN27 Sample Name: blu t360 e60 Misc Info: Vial Number : 8 r Analyse quantitative : Testosterone/Epitestosterone r ! ■ n i \ r'i LI SI :METHYLTESTOSTERONE r'l U u '^Tiite TIC: REF3TE.D 600000 500000 400000 300000 200000 A 100000 nme-> 5. . 1 , , .. , ' 1 .. .J X 10.00 ■■■(■■■■ 15.00 2 1 0.00 Abundance Iwi 301 .30 (301 .00 to 302.00): REF3TE.D 2C192 140000 120000 100000 80000 60000 40000 20000 2^&a»S3 I nme-> 20,50 21.00 21.50 22-00 22.50 Epitestosterone- Testosterone \bundance 500000 400000 300000 200000 100000 Ion 432.40 (432.10 to 433-10): REF3TE.D 19|32 18,52 18. iB.g8 ' ' I ' ' I ' I 18.50 19.00 ig.SSlBSQ.m.27 19.50 20.00 20.S -n 20.50 Epitesto-Testo-llbetaOH A et E Miundance 500000 Ion 432.40(432-10 to 433.10): REF3TE.D Ion 522.50 {523Sla&i 523.20): REFSTE.O 400000 300000 200000 100000 18.52 1^ 1B.4Q 18.98 19.(ISIB3Q.Q9.37 20i 1 1 1 1 'l 'i 1 1 1 1 1 1 'i 'j 1 1 1 1 1 1 1 1 I 1 ) 1 1 1 r [ 15.50 19.00 13.50 20.00 20.50 page 1 USADA 0096 S^ L, ' n n L.l r Li u a LJ D ] LNDD ENREGISTREMENT Codification: E-CC-11 Version : B Date: 08/03/2006 1/1 VERIFICATION DES PERFORMANCES INSTRUMENTALES EN CG/SM (screening et confirmation) Niim6ro d'identification de I'appareil : P^DS^O "Date: ^0^06 1 - Source d'topisation MSD Autotune: Ion 69 ou 219 majoritaire Autotune- : Abondance de I'ion 502 > 3% Repeller<35 Polaris Ion time > 2 ms ■ Observations :. 2 - Etancheite du svstSme MSD / 1 S/69 ( H20), 28/69 (N2}, 32/69 (02), . , 44/69 (002) < 10% Polaris ■ . Air et eau : Intensity ion 19 < ' intensity ion 18 Observations : 3 - Sensibility Oui Non y V X Oui -Non ^ Oui Non Screening Recal / Mix confoime _^ i — a Conf TP confortae-Fichier : ~^ "^ ^ ^ < TT confonne - Fichier ; . TP confoime ~ Fichier : TP confonne - Fichier: TP confoime - Fichier: Observations : ] Code op6rateur et paraphe : 't^ro, U(y Cet enregistrement est a archiver dans h classeur C-MA-Ech de I'appareil USADA 0097 Zl 5973 Autotune ^ ^ n ! ■L r] u u . [ ' I L.J a Instrument: MSD 20 Hon Jul 24 11:14:38 2006 D:\MSDCHEM\1\5973N\ATUNE.U Mass Ab Pw50 69.00 442402 0.62 Mass Ab PwSO 215.90 243594 0.62 Mass Ab PwSO 502.00 16830 0.63 Ion Pol POS MassGain MassOff s Emission 34.6 AmuGain EleEnergy 69.9 AmuOffs Filament 1 Wid219 - DC Pol Repeller 29.79 lonFocus 90.2 HED EntLens 11.5 EMVolts EntOffs 19.33 Samples PFTBA OPEN Averages StepSize Zones : MS Source 230 Foreline MS Quad 15 397 -10 2576 127 0.018 NEG ON 1353 B 3 0.10 61 1 -^ . - k . \ 1 ' ' 1 1 ' 1 ' ' 66 71 216 . 1 1 . 1 . 1 . . 1 221 500 505 Scan: 10.00 - 700.00 Samples: 8 Thresh: 100 Step: 0.10 127 peaks Base: 69.00 Abundance: 397824 uu - 80 - 60 ■ 40 - 20 - , 1. . 1 1 .i.. U -' 1 ' — ^r-* ' i" y'^l — ^ ' ' 1 ' 1 ' ' 1 ' ' ' ' 1 ■ ■ ■ ■ 1 ■ ■ ■ ■ 1 100 200 300 400 500 600 Mass Abund Rel Abund Iso Mass Iso Abund Iso Ratio 69.00 397824 100.00 70. 00 4362 1.10 219.00 225088 56.58 220.00 9995 4.44 502.00 15492 3.89 503.00 1554 10.03 USADA 0098 ?>?> 5973 Air and Water Check F^i n Li ri Li n t : r u LJ UJ Lv D u LJ Instrument: MSD 20 Mon Jul 24 11:16:34 2006 D : \MSDGHEM\ 1 \ 5 973N\ATUNE . U Scan: 10.00 - 75.00 Samples: 8 Thresh: Step: 0.10 65 peaks Base: 69.00 Abundance: 492B00 uu - 90- 80- 70 - 60- 50- 40- 30- 20 - 10- n 1 ,1 1 u - — 1 — 1 — 1 — ^-f — — 1 — 1 — 1 — 1 - — T — M — — 1 1 — -T- — 1 — -| r r ■ ' f 1 1 T" ■ 1 1 1 1 r 1— 1 ' ' 10 20 30 40 50 60 70 Mass Abund Rel Abund Iso Mass Iso Abund Iso Ratio 69.00 492800 100.00 70.00 5635 1.14 18.10 7001 1.42 18.90 65 0.93 28.10 27608 5.60 29.00 335 1.21 Current Params used: Rep =29.8 Entl = 19.33 Entr = 12 FOCUS = 90 EMV = 1353 Relative abundances : 18/69 = 1.42 28/69 = 5.60 32/69 = 1.69 44/69 = 0.13 28/18 = 394.34 Water% Nitrogen% Oxygen% Carbon Dioxide% Nitrogen/Water% USADA 0099 30 n File: D:\Msd20\juilO6\2407\TPlTE.D Operator: 2 8 Date Acquired: 24 Jul 2006 11:55 Instrument: MSD 20 Method File: MaN27 Sample Name: tp te2 Misc Info: Vial Number : 2 U Analyse quantitative :Testosterone/Epitestosterone \ [ L. n u D Abundance TIC:TP1TE.D 600000 500000 400000 300000 200000 1DOO0O ^ J. 1 . ilwJu— t .i-jlli 11- .|M J I. oiUt J Of rime-> 5.0 10.00 1 1 1 1 I 1 I 15,00 1 1 ,— , — , 20.00 ' Epitestosterone-Testosterone \bunigj^ Ion 432.40 (-132.10 to433.10}:TP1TE.D 19.33 [ 5000 4000 1 18.' 3.53 3000 2000 19.68 1000 -J 18.9S \MMJi r. u rime-> 18.50 19.00 19.50 20.00 20,50 SI :METHYLTESTOSTERONE Abundance 200000 150000 100000 50000 Ion 301.30 (301 .00 to 302.00); TPJTE.D 2CL95 1.0420.36 ri[ne-> |i jr^^i |i i | 1,1 ;.i | ^ ^-p.p jy^ j - ,.. p, I " I I I I T T [" I "!' ! I 20-50 21.00 21.50 22,00 22.50 Epitesto-Testo-llbetaOH A et E ^bundance lon432.4O(432.10to433.10):TPlTE.D ''^■^ Ion 522.50 (522.20 to 523.20): TP1TE.D 13.33 5000 4000 3000 rime-> 18.53 18.4 ! I ' ' ' ' I ' ' I ' I ' ' ' ■ I" ' I I ' I ' ' I ' I 1B.50 19.00 19.50 20.00 20.50 J page 1 US ADA 0100 2^. r ■; { [J r r I I LI i"l J I L- r 1 G [J LNDD ENREGISTREMENT Code: Version : Date: FICHE D'ANALYSE / RESULTAT - CONFIRMATION SEMI-QUANTITATIVE T/E E-FCR-04B E 29/05/2006 1/1 Paraphe: f^C-' Echantillon : 178/07 995474 Zl Dilution : 1/ 1 Ion de quantification Testo etEpitesto : Concentration de la reference 1 Concentration de la reference 2 Concentration de la reference 3 432 Testosterone: Testosterone: Testosterone: Ion de quantification SI : 30 Epitestosterone : 180 Epitestosterone: 360 Epitestosterone : 301 5 30 60 T/E theorique : 6 T/E theorique ; 6 T/E theorique : 6 Fichier Surface du SI Surface Testosterone Surface Epitestosterone REFl REFITE 5915926 1557516 234336 REF2 REF2TE 4981326 7052377 12H449 REF3 REF3TE 5130998 17023691 2929592 17807474 6399496 3513238 307234 RESULTAT DE L'ECHANTILLON Valeur obtenue Valeur finale Concentration Testosterone 61,4 nfi/mL 61,4 ng/niL Concentration Epitestosterone | Rapport T/E en surface 5,2 Partie a rempiir par le responsable Seuil de declaration du rapport T/E ( en surftce) : 4 Incertitude (liee a la methodc) pour le rapport T/E : 2>C?/; pour Epitestosterone : "iO^ pour la Testosterone : -204 Valeur basse du rappori T/E : *? Valeur haute du rappori T/E : I U •■ tS ■. Resultat: Anormal : o^ Inclassable : Negatif : Correction des concentrations en Te§tosterone et Epitestosterone par la density (cf doc E-nvC-fll) : Densite affichee Numiro du r^fractometre Densite corrigfe : Facteur de correction Cop centra tion corrififa de Testosterone ConcentratioB corrlgfe d' Epitestosterone ^ rv9S ^ £>^^ fi^IT ti^.^ :2ua PARAPHE e Ecart n° : Cel enregislremeni est a archive)- dans le dossier de confirmation USADA 0101 5iA