.^i^e= C:\MSD18\JUILLET06\2107\21hO8.D\da Operator: Tn37p35 ^ Date Acquired: 21 Jul 06 7:36 pm . Instrument; GC MSD ,. Method Pile; MAN06B_B.M Sample Name: 178/07 995474 H Misc Info: Vial Number : ii ■'"'^ ^'^EA PrSgnanediol llKetoetiocho land one Abundancelon 434.40 (434.10 Abundancelon 432 40 (432.10 Abundancelon 117-10 (116-80 Abundaneelon 343.30 (343.00 600 400 2O0 lnie~> 14-00 '; .. A 1000 14.87 Time-> 13.40 14.10 Time-> 17.00 4000 3000 2000 1000 u.p 17-86 Time-> 14.00 14.87 .b Androstandione 4 Androstenedione Inhib derivation 3a-5 Cyclo Jjundancelon 432,40 432-10 Abundancelon 430.40 (430-10 Abundancelon 36 UO (36100) Aliunclanceion432-40(432.10 1500 1000 SOD 11.E30 800 600 400 200 3000000 rime--* 10-30 11.60 Time-> 14.00 15.30 Time-> 150 Tlme-> 9.00 Page 2/16 USADA 0056 5-/ D:\mKl1 91Jull07U!507\17807474.D Data File Path O;ViT>sdi9\)utiO7\250n Data File Name 17807474.D Operator M45P35 Acq. Method File MAN06B_B.M Sample Name 178/07 995474 H Misc Info Vial Number 2 Instrument Name MSD19 Calibration Title Calibration des stdroides endog^nes Last Calibration Update Tua Jul2S 15:15:32 2006 Fichierrecal utilise 25rcl01.D Dale : i.'S\,oi\pjC., Op6rateur : .lO, C[] R^sultats : HC[] N6gatif A v6rifier [} [] Remarques : ......^. .J2a..Sc/Li2MXjS 1 # Pealt Type Ret Time Signal Name Target Response Amount Units 1) •ISTD 17.14 301.3 Methyltestosterone 1,731.969 100 ng/ml ■I) 12.38 438.4 Andro -04 glue 104,768 170 ng/ml 3) 0.00 372.3 Salbutamol -D3 ng/ml 4) 12.41 434.4 Androsterone 9,973,015 1658 ng/ml 5) 12.64 434.4 Etiochoianolone 11,119,071 1639 ng/ml 6) 12.78 241.2 5a33 diol 524,770 97 ng/ml 7) 12,94 241.2 5b3a diol 1,240,694 227 ng/ml 8) 17.79 117.1 Pregnanediol 19,393,646 487 ng/ml 9) 0.00 434.4 DHT ng/mi 10) 13.81 432.4 DHEA 151,077 21 ng/ml 11) 14.35 432.4 Epitestosterone 214,591 11 ng/ml 12) 15.23 432.4 Testosterone 1,093,773 50 ng/ml 13) 0.00 371.3 THC-M ng/ml 14) 0.00 369.3 Salbutamol #DIV/01 ng/ml 15) 15.98 522.5 1 1 bOH Etiochoianolone 554,334 130 ng/ml 16) 21.35 548.5 THS 1,376,986 88 ng/ml 17) 22.11 636.6 THF 32,301,427 2915 ng/ml 18) 22.85 632.6 Cortisol 1,008.236 143 ng/ml 19) 14.73 343.3 11 Ketoetiocholanonlone 2,541,956 309 ng/ml 20) 0.00 241.2 3a-5C ng/ml [Surface] [concentration] Valeurs conventionnelles de relet Ad4alu/Si'10D 6.0 <12.9 T/ET 5.1 Rapport >4 Testosterone 49.7 Concentration >200 Epitesto 11.1 Concentration >200 Androsterone 1,658 Concentration. > 10000 Etiochoianolone 1,639 Concentration >1O0O0 DHEA 20.6 Concentration >200 DHT 0.0 Concentration >20 Andro / Etto 0.9 Rapport >3 5a3a/5b3adiol 0.4 Rapport >2 THC -M 0.0 Concentration >15 Salb/SalbD3*100 #DiV/0! #DiV/0! Concentration >75 Cortisol /THS 1.6 THF /THS 33.1 llbOHetio/THS 1.5 Pour info (R&D) THF 2915 Sl/3a5c #DIV/0! USADA 0057 55 ^ile: D:SMSD19\JUIL07\2507\17807474.D\da Operator: M45P35 Date Acquired: 25 Jul 06 10:'52 am Instrumenc: MSD 19 Method File: MAN06B_B-M Sample Name : 178/07 995474 H Misc Info: Vial Number : 2 Andro ~DA glue Abundance 8000000 6000000 4000000 2000000 TIC: 17a07'174.D\daasim.ms Methyltestosterone Abundariceion 438,40 (438.10 to 439i [Abundance Ion 301,30 (301,00 to 302. 11.789 i : i Time-> 5.00 i 20001 1000! i2..a8i: : \' I 17,139 200001 lOOOOi ^m'■ 10-00 15.00 20.00 25.00 irime-> 11.50 12.00 '- ' \- rirne--> 16.00 16.5017.0017.50 Salbutamol -D3 Cortisol D4 Adundancelon 372.30 (372,00 to 37 Wiundancelon 636.60 (636.30 to 62 ^undancelon 434.40 (434 10 to 4: 3.970 200ol Andro-Etio dl TtviS Andro-Etio mono TMS 1000' ! :|. ■■J - I, - ' ■ I ' ■ 0- Time-> 4.00 4.50 ^^JUIIUdNUe IDII t>x .DJ ( }Jt> JU ID OJ 10000 5000 frime-> /J V u -/^ ^-.^_' 23.00 ' ' 1 rime-> 12.50 \bundancelon 272.20 [271 ,90 to 2^ 600000 loK^tSO (362.00 to 36 400000 200000 11.127 nmB-> io.79a'inji' 192 293 10.50 11.00 5a3a-5b3a Diol si 5b < trait : IRM S Epitestostferone - Testosterone THC -M 10000 0— Time~> 12.50 13.00 : [nme-> 14.00 14.20 14.40 14,60 14.80 15.00 15.20 15.40 Cortisol THF THS toundancelon 632.60 (632,30 to 63 Abundancelon 636.60 (636,30 to 63 |^twndancelon 548,50(548,20 to 5- 60000 40000 20000 22.852 i 22B.ta9 Time-> 23.00 1500000 1000000] I 500000 I i oi Tinr»-> 22,1 22.00 11 BOH A/E ^bund3nce 40000 Ion 522,50 (522,20 to 51 15*84 30000 20000 10000 , j^ 15,SS0 1 Ui — 1 — -- — -— ' — 1 — . — • — . p nme-> 15,50 16,00 ■-\ Page 1/16 US AD A 0058 53 Tile: Opei?aEor : Date Acquired : Instrument : Method File : Sample Name r Misc Info: Vial Number : 2 °"'^ . DHEA P r^gnanediol l lKetoetiochola noione Abundancelon43440(434.10to4; Abundancelon432.40 (432.101o4; Abundancelon 117.10(116,3010 11 Abjnflancelon 343.30 [343.00 To"34 D: \MSD19\JUII.07S2507\17807474.D\da M45P35 25 Jul 06 10:42 am MSD 19 MAN0 6B_B.M 178/07 995474 H 14.724 2000 1000 4000 2000 13.808 300000' I 200000] 100000 14.733 0-^ Time-> 14.00 17,800 1 17.6B6' i 40000' 20000 14.50 ; rrime-> 13.50 14.00 irime-> 17.30 14,302 nnie-> 14.00 14.50 ^^ Andres tan d lone 4 Androstenedione Inhib derivation 3a-5 Cyclo A&undancelon 432.40 [432,10 to 41= Wundancelon 430.40 [430.10 to 42 Abundancelon 361,30 (361,00 to 3E 'Abundancelon 432,40 [432,10 to 42 2000: 1000 11.273 11.161 Tin>e-> 10,50 11.00 11.50 4000 9, 63 i 3000 2000 8,827 h 1000 Alj^-'UAN'' rime-> 9.00 9.50 Page 2/16 USADA 0059 ^^ C:\MS D1 BUUlLLETaE\2107\21rcl03.D 5ata File Path C:\MSDiBUUiLLET06\2ion Data File Name 21rcl03.D Operator Acq. Method File MAN06B_B.M Sample Name 2107 rcl 028 2007 HI Misc Info Vial Number 1 Instrument Name GC MSD Calibration Title Calibration des steroides endogenes Last Calibration Update Fri Jui 21 13;26:58 2006 FictiJer recal utilise 21rcl03.D # Peak Type Ret Time Signal Name 1) •ISTD 16.99 301.3 Methyltestosterone 2) 12.21 438.4 Andro -D4 glue 3) 4,08 372.3 Salbutamol -03 4) 12.22 434.4 Androsterone 5) 12.47 434.4 Etiocholanolone 6) 12.61 241.2 5a3a diol 7) 12.77 241.2 5b38 dioi 8) 17.60 117.1 Pregnanediol 9) 0.00 434.4 DHT 10) 13.65 432.4 DHEA 11) 14.22 432.4 Epilestosterone 12) 15.10 432.4 Testosterone 13) 17.36 371.3 THC-M 14) 4.10 369.3 Salbutamol 15) 15.83 522.5 11 bOH Etiocholanolone 16) 21.29 548.5 THS 17) 22.04 636.6 THF 18) 22.80 632.6 Cortisol 19) 14.57 343.3 1 1 Keloetiocholanonlone 20) 0.00 432.4 3a-5C Date:.^41.U&,. Operateur ; ...23::.. CM Resultats : Hcn Ndgatif A verifier [] Remarques : Target Response Amount 1,587,292 200 62,992 125 472,321 100 9,682,254 2000 9,908,352 2000 268,022 100 257,498 100 4,046,186 400 457,571 100 446.439 40 498,991 40 49,013 15 443.177 94 923,980 200 585,640 50 16,444,095 1500 473.452 50 369.571 100 Units ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml ng/ml Ad4glu/Si'100 T/ET Testosterone Epitestosterona Androsterone Etiocholanolone DHEA DHT Andro / Etio 5a3a / 5b3a diol [Surface] THC -M Salb/Salb 03 ' 100 Cortisol / THS THF / THS 11 bOH etio /THS THF Sr/3a5c 4.0 1.1 [concentration] 1.0 1.0 94 #DIV/0! 40.0 40.0 2,000 2,000 100 15.0 93.9 1.0 30.0 4.0 1500 Valeurs conventionnelles de relet Rapport Concentration Concentration Concentration Rapport Rapport Concentration Concentration <19.1 >4 >200 >200 Concentration > 10000 Concentration > 10000 Concentration >200 Pour info (R&D) >20 >3 >2 >15 >75 USADA 0060 5! C:\MSDlB\JUrLLET06\2107\21rcl03.D\da File: Operator : Date Acquired: 21 Jul 06 12:59 pm Instrument: GC MSD Method File: MAN06B B.M Sample Name: 2107 rcl 025 2007 HI Misc Info: Vial Number : 1 Xbundance 1000000 500000 i I TFC: 21fcl03,DUaUsini.ms ^ ■■■ ■lme~> 5.00 ^..^ Andre -D4 glue Methyl testosterone Abundancelon 43S.40 (438.10 to Abundancelon 301.30 (301.00 to 12 '13 1000 / 500 1 U ' ' ■ ' ■ 15.00 20,00 25,00 Time-> 11.50 12,00 16. 191 30000 20000 10000 . 1 1 ■ ' ■■""■ — Tlme-> 16.00 17,00 10.00 "albutamol -D3 Cortisol D4 Andro-Etio di TMS Andro-Etio mono TMS : bundancetan ajZ-SO (372.00 Abundancelon 636.60 (636.30 Abundancelon 434.40 (434.10 Abundancelon 272.20 (271 .90 1000 20000 15000 1OOO0' SOOQ 4. 82 500 rime-> 4.O0 -J ^-^■K^--.^ 200000 150000 100000 50000 4.50 Time-> 22.50 12ilS.471 150O 1000 500 23.37 Time~> 12.00 12.87 Time~> 10.00 11.30 3a3a-5b3a Diol .;i 5b < trait : IRMS EpitestostSrone - Testosterone THC -H \bundancelon 241 .20 (240.90 Abundancelon 432.40 (43210 to 433,10); 21rd03.D\daUslni.ms Abundancelon 371.30(371.00 aOOOj 12p6g 60001 11 4000 2000 10000 5000 ■ime-> 12.30 Cortisol 13.17 TimB-> 14.00 14.20 14.40 14.60 14,60 15.00 15.20 15.40 Time-> 17.00 1000 500 / y\ . ' ' 1 17.66 THE THS 11 BOH A/E Abundancelon 632.60 (632.30 Abundancelon 636.60 (636.30 Abundancelon 548.50 (548.20 Abundancelon 522,50 (522,20 30000 1 20000 10000 01— r ■■■■ne-* 2Z.50 1000000 22, Ml 500000 ' 1 30000 20000 10000 40000 30000 20000 10000 23,37 Timo-> 21.50 22,37 Time-> 21.00 Page 1/16 15,629 21.86 Time-> 15,30 16,17 US ADA 0061 3G C:\MSD18\JUILLET06\2107\21rclO3.D\da File: Operator: Date Acquired: 21 Jul 06 12:59 pm Instrument; GC MSD Method File: MAN06B_B.M Sample Name: 2107 rcl 028 2007 HI ' Misc Info: Vial Number : i ^r^M , .,,>., ^"^ Pregnanediol llKetoetiocholanolone -bundancelon 434.40 (434.10 Abundancelon _432_.40 (432.10 Abundanceion 117.10 (116.80 Abundancelon 343.30 (343.00 )4.j|l24 3000' 20001 1000 '14.217 I i 10000 5000 13*52 W ..„ Trme-> 14.00 60000 60000 40000 20000 17i96 I 14.86 Time-> 13.40 / A , , 8000 i 6000 4000 2000 'T 14.10 Time"> 17.00 17.B6 Time~> 14.00 14.86 3b Androstandione 4 Androstenedione Inhib derivation 3a-5 Cyclo ^bundancelon 432.40 (432.10 Abundancelon 430,40 (430,10 Abundancelon 361,30 (361.00 Abundancejon432,40(432,10 1000 500 100 50 .'ime-> 10.30 11,60 Time-> 14.00 300 200 TOO r^ it^NfM 40 20 15,30 Time-> 5,50 6.00 Tf[ne-> 9,00 Page 2/16 USADA 0062 <=;:i LNDD ENREGISTREMENT Codification : E-CC-11 Version : B Date : 08/03/2006 1/1 VERIFICATION DES PERFORMANCES INSTRUMENTALES EN CG/SM (screening ef confirmation) Num6:o d'identification de I'appareil : HJ^ ^ s Date: J\\'^\c^ 1 - Source d'ionisation MSD Autotiine : Ion 69 ou 219 majoritaire Autotune : Abondance de I'ion 502 > 3% Repener<35 Polaris Ion time > 2 ms Observations : Oui Non X X X 2 - Etanch^Re du svst^me MSD Qui Non 18/69 ( H20), 28/69 (N2), 32/69.(02), 44/69 (C02)< 10% Polaris Air et eali : Intensity ion 1 9 < intensite ion 1 8 Observations : r^ 3 - Sensibilite Screening Conf Recal / Mix conforme TP conforme - Ficliier TP conforme - Fichier TP conforme - Fichier "TP coufoime - Ficliierr TP conforme - Fichier: Observations ; Oui Non ^ Code operateur et paraphe : ^ cSlcSi^loW Cei enregistrement est a archiver dans le classeur C-MA-Ech de I'appareil USADA 0063 55^ "I .:iSD18\juilletO6\2107\21rcl03.D ; 21 Jul 06 12:59 pm ame : 2107 rcl 028 2007 hi VERIFICATION DU RECAL ANABOLISANT J'e«iT"' i„°'u^r?f iLXpt'^fr'^'^' w -« ..A.„...,..,„ „„.Xa«..,.3.so ^^L{,L, li%%.^,i,,^ 1000 JOQI I 7 ■ 500 l\ ^^..j^ -~-.-2 is^n:i£.oa.«;S laris:::"^ 200 500 . Si^^..«HiS:!J ssis.»..,s ssiswS j™::::^ 400 200 or™:-^,^- Tlm<^ 10.00 loW Time->2230 22.74 Time-> 11.00 200 11.87 Tlme-> 17.00 17.86 I ■ I . IDate iOpSrateur IR^sultats 1 1 ! Remarques ^^&£ .Q Conforme Kd ! Non conforme USADA 0064 ^^ ^'1 Fri Jul 21 10:50:37 2006 C : \MSDCHEM\ l\5973N\atune . u Mass 69.10 r Mass Ab 402237 Ab Pw50 O.Gl PwSO I 5973N Autotune Instrument; GC MSD 219.00 353944 0.60 Mass 502.10 Ab 70474 PwSO 0.59 '•A. Ion Pol Emission EIEnrgy Filament Repeller lonFcus EntLens EntOffs PFTBA POS MassGain -les MassOffs -11 34 . G AmuGain 69.9 AmuOffs 2 Wid219 DC Pol 34.81 90.2 HEDEnab 9.5 EMVolts 18.32 Samples 8 OPEN Averages 3 Stepsize o.io 1830 135 -0.038 POS ON 171B Zones : MS Source MS Quad 230 Foreline 150 66 71 216 221 500 505 Scan: 10.00 - 700.00 Samples: B Thresh: 100 Step: 0.10 137 peaks Base: 69.00 Abundance: 387776 100 80 - 60 40 20 .^J... .■ I ,■> ' > 100 200 300 400 500 600 Mass Abund Rel Abund Iso Mass Iso Abund Iso Ratio 69.00 387776 100.00 70.00 4355 1 12 219.00 341120 87.97 220.00 14592 4.26 502.00 67320 L7.36 503.00 6523 9.69 Air/Bater "uneck: H20-0.&S%/ N2-J .61* 02-1. 00* — C02-Q.i6% M2/HS6~3eO.S 7 t Column Flow; Front: 1.324 Back: ml/min. Interface Temp: 300 Ramp Criteria: Ion Focus Maximum Repeller Maximum 90 volts using ion 502; 35 volts using ion 219; EM Gain 80957 MassGain Values ©Samples: -18703 -17902 -17181 -157®0 -113@PS 72 TARGET MASS: 50 69 131 219 Amu Offset: 135.0 135.0 135.0 135.0 Entrance Lens Offset: IB. 3 18.3 18.3 18.3 414 135.0 18.3 502 135.0 18.3 800 135.0 18.3 USADA 0065 6o : latefttquired .•ample name C:\MSDie\juillet06\2107\21cq01.D 21 Jul 06 3:06 pm 2107 cq 028c 2107 HI 1 VERIFICATION DU CONTROLE QUALITE AKABOLISANT L9 Norajidrosterone 3' OH. atanozolol Salbytamol Clost^bol -M Pre [X, '^s [ ) Pre ^ Abs [ ] Pre Wy, Abs [ ) Pre (X Abs [ J Abundancelon 422.40 (422.10 Abundancelon 254.20 (253.90 Abund^ceion 369.30 (369.00 Abundartcelon 451 40 (451 10 > , I I 200001 I I t I 400OI 1 ! I 10000: soooi li 2000 10000 1000 0| . ■ ■'. ^-. -T - oF^-- .-- .-^^^^i^^F ol < . V ' ^ i. T 'i- ririte~> 10.00 10.87 Tlme~> 22.30 22.74 Tifne-> 4.00 4.50 Time-> 15.50 16 37 ^bundancelon 405.40 (405.10 Abundancelon 545.50 (545.20 Abundancelon 86.00 (85.70 to Abundancelon 466 40 (466 10 ' ' 20000 1000 500 5000 0[ ■me-> 10.00 10000 oH^ >-- ■/^ 1000 500 10.87 TJme-> 22.30 2274 Time-> 4.00 4.50 Time->15!50 16 37 aundancelon 420.40 (420.10 Abundancelon 560.50 (560.20 Abundancelon 440.40 (440.10 Abundancelon 466.40 (468.10 500 ^^. V^_vn„,...-' 4000 2000 Vvj nfne~> 10.00 10.67 Time-> 22.30 ?re [y^RJos [ ] Xbundart^elon 223,20 (222.90 100000; 500001 ; 0^' . I . . . . r-^ :me-> 3,20 3.40 bundancelon 294.20 (293.90 -■.: 4OO00 I 500 rime-> 15.50 16.37 BupSe no r ph i ne Pre [yO Abs [ ] Abundancelon 554.50 (554.20 Abundanfcelon 372.30 (372.00 ZOOO 40''" 1000 0f= 20O0O o ' n Time~> 23.00 23.87 Time-> 4.1)0 Abundanceton 506,50 {506.20 Abundancelon 66.00(85.7010 200001 r 1000 Jx.,... r 'me-> 3.20 3.40 -abundance Ion 295.20 (294.90 ■ 40000 20000 20000 10000 Time-> 23.00 23.87 Time-> Abundancelon 450.40 (4S0.10 1000 Ol-r- 4.00 500 0' . ■■. . ,T :ime~> 3.20 3.40 Time-> 23.00 23.87 IDate !Op€rateur IRSsultats I 1 ! t Remarque a [ .^.l^lofe,.^ ■ ■■?V-f^& Conf orme X^ Non conforme { ] :Qi^^ USADA 0066 GJ Abs [ ] Pre [oi^ Abs 1 ] Pre p< Abs [ ] Pre [^Abe [ ] ^bundancelon 422.40 (122.10 Abundancelon 254.20 (253.90 Abundance on 369.30 (369.00 Abundance 1*451.40(451.10 10000 5000 .-.-^- 4000 2000 ^- 1D00O -W 1000 500 ■nmp >10 00 1087 Tinie->2230 2274 T\me-> 4.00 4.50 ■nme-> 1S.50 16.37 Abundancelon 405,40 (40510 Abundancelon 545.50 (545.20 AbunOancelon 86.00 (8570 to Abundancelon 466.40 (466.10 lOOOl [l ' 5000 10000 V 1000 500 ime->1000 10:B7 Time->2230 2274 Tims-> 4.00 4.50 Time-slsiSO „ „l^-3j' :.bundance'lon 420.40 (420. 10 Abundancelon 560.50 (560.20 Abundance on 440.40 (440.10 Abundancelon 4M.40 (466,10 500 A f\, 4000 2000 /'wvj 1000 ^ L^. 400 200 ,"ime-> 10.00 10.67 ■nme->2130 22,74 Time-> 4.00 4.50 Time-> 15.50 16.37 Bupr e norphine Pre [^Abs Sij Sthamivan j>re [ (V Abs { ] \bundanceion 223.20 (222-90 Abundancelon 554.50 (554.20 Abundance on 372.30 ■ 1OO0O0 Salbutamol D3 Pre 04 Abs [ ] 372.00 5O0O0 .lme-> 3.20 J 2000 1000 3.40 20000 ime-' 0.6U o.-- Trme-> 23100 23.B7 Tlme-> 4.00 bundancelon 294.20 (293.90 Abundancelon 506.50 (506.20 Abundancelon 86.00 (85.70 lo 40000 ' 20000 rJ 1000 T 10000 .*ime-> Z20 3.40 Tlme-> 23.00 23.87 Time- '.bundancelon 295.20 (294.90 Abundancelon 450.40 (450.10 1000 4.00 20000 .ime-> 500 |-,->-^-pr-r 3.20 3.40 "nme-> 23.00 23.87 IDate lOpSrateur !R6sultats ! Remarque s : I I 1 . ma^o^. Conforme [SO Non conforme [' ] " '-o^-- USADA 0067 6Z LNDD ENREGISTREMENT Codification : E-FSR-01 Version : G Dale 22/03/2005 FICHE D'ANALYSE / RESULTAT DEPISTAGE RAFIDE CG/SM, CG/TSD ET CL/SM Echantillon : Produit suspect^: 178/07 99S474 U .'It'estosterone .r&. Tolerance interae sur le Ir et le trr en intrajour : +/■!% {si tn < 0,6) ou +/-0,5% (si trr > 0,6) Tolerances internes sur les abondances relatives en intrajour : Plage d'abondance Tolerance CG >50% +/-50%(cnreiatif) 25 ■ 50% +/- 50% (en relatif ) <25% +/- 50% (en relatif) Tolerance CL +/-15%(enabsolu) +/- 25% (en relatif) +/- 10% (en absolu ) Rg__: en CG, si I'lgn a une atondMce <10%, seule la prfaCTce de I'ion sufBt. Echantillon Reference intrajour Reference int«}our Fichier : 21H08 21rcl03 wMW^BIM^E SSSSSSWHWIB Tolerance basse Tolerance haute Tolerance basse Tolerance haute tr 14,300 min 14,220 min 14,149 min 14,291 min min min trSl 17,090 min 16,990 min ^^^M Bmm Hgg nmud trr 0,837 0,837 0,833 0,841 Ml 100,0 % too.0% illl^ ^^^■HHHJ^^^H M2 M3 Les tolerances sont calculi par rapport k la reference ConcOTdance des tr : Oui Concordance des trr : Oui Concordance globale des abondances relatives : Oui Parapbe et code op^ateur ; \^ ^ ^ Nmi Non Nod ^ I r r r Partie h remplir par le responsable A confirmer : Parapbe du responsable ; Obsnvations : Oui ^J £ Non Cet enregislremeni est k arcbiver dans le dossier de la s^rie ( si pas de confirmation) ou dans le dossier de confirmation USADA 0068 f^2 LNDD ENREGISTREMENT Codification : E-FSR-01 Version : G Date 22/03/2005 FICHE D'ANALVSE / RESULT AT DEPISTAGE RAPIDE CG/SM, CG/TSD ET CL/SM ■ 1 "I E chant i lion : Produil suspect^: 178/07 995474 Testosterone Toferance interne sur'le tr et fe tn en Intrajour ; +/-!% (si trr < 0,6) ou +/-0,5% (si trr > 0,6) Tolerances internes sur les abondances relatives en intrajour : Plage d'abondancc Tolirance CG > 50% +/- 50% (CD relatif ) 25 - 50% +/■ 50% (en relatif) <25% +/- 50% (en relatif) Rg^: en CG, sH'ion a une abondance "^ tO%, se ule l a pre s ence de I' iqn suffit. Tolerance CL +/-15%(enabsolu) +/- 25% (ra relatif) +/- 10% (en absolu) Echantillon Reference intrajour Reference inlerjour Fichier : '-il'i-W'MJIrr^YiiHtfrlTf 21H08 "-^1 1 ini'ihi'iT 1 iThkit AJIhU^ahSMIBB^gEaMB 21rcl03 tr 15,200 min 15,100 min 1 UlClaiJHJC UkqC 15,025 min 15,176 min min min trSI 17,090 min 16,990 min WBMBS SBBH BBBBHBI trr 0,889 0,S89 0,884 0,893 Ml 100,0 % 100,0 % BMHH HHH ■MHIld M2 M3 Les tolerances sent calculto par rapport il la r^f^ence Concordance destr : Oui Concordance destrr : Oui Concordance globale des abondances relatives : Oui Par^he et code opirateur : — /^ :s Non Non '^ A continner : Paraphe du responsable : Observations ; Partie k remplir par le rcspcHisable Oui I oi I Non <£ Cel enregistrement est a archiver dans le dossier de la s^rie ( si pas de confirmation) ou dans le dossier de confirmation USADA 0069 6^ r-\ ^^ -^ ■^ I 1 SECTION! TECHNICAL PART 2.3 Second analysis for confirmation of T/E ratio ~-, !J i ■ J USADA 0070 LNDD ENREGISTREMENT qiSTE) Codification : L-CONF-01 Date : 09/06/2006 1/3 C p EC ^^AEN LISTE DES CONFIRMATIONS REALISEES AU LABORATOIRE ^^^^^'^^^ QUALIT Produits confirmes Stimulantsf*) Methylamphetamine Fonnes L et D de I'Amph^tamine et de la MethylamphetamiDe Amines (*) primaires par CS2 Amines (*) primaires par CS2 Amines {*) primaires par CS2 I Surveillance AMA : Cafeine Quali ephfeirines Quanti ephedrines Quanti Norephedrines Surveillance AMA : Ephedrines Essai EC08 EC09F EC57 ECU ECllA ECIIB EC13A ECI3B EC13C EC13D Instractions I-CONF-08 I-CONF-09F I-CONF-57 I-CONF-11 I-CONF-llA I-CONF-1 IB I-C0NF-12C I-C0NF-13A I-CONF-1 3B I-CONF-1 3C I-C0NF-13D Mod op extraction M-EX-OIB M-EX-02D M-EX-57 M-EX-05 M-EX-05A M-EX-05B M.EX-06 M-EX-08A M-EX-08B M-EX-08A M-EX-08A Mod op analyse M-AN-02 M-AN^2 M-AN-57 M-AN-12 M-AN-12B M-AN-12B M-AN-02B M-AN-14 M-AN-15 M-AN-16 M-AN-14 Type d 'analyse GC/Quad (SCAN) GC/Quad (SCAN) GC/Quad (SCAN) GC/Qiiad (SCAN) GC/Quad (SCAN) Gacjuad (SCAN) GOQuad (SCAN) GC/Quad (SCAN) GC/Quad (SIM) GC/Quad (SIM) GC/Quad (SCAN) Betabloquants C*)par MBA B^tabloquants (*) par MBA (sans hydroiyse) EC14A EC14B I-CONF-1 4A I-CONF-1 4B Atenolol I Stupgfiaiiis (*) M-EX-09 M-EX-09 Etilefrine M-EX-56 M-AN-17 M-AN-17 M-AN-56 GC/Quad (SCAN) GgQuad (SCAN) GOQuad (SCAN) HPLC/MS3 ESI Etilefrine Hydromorphone EC09D I-CONF-09D M-EX-02E THC-M Clocaine-M Quali moiphine Semi quanti Morphine surveillance ministfae EC09C I-CONF-09C EC09E I-CONF-09E EC25 I-CONF-25 Quanti morphine EC27B I-CONF-27B M-EX-20 EC26 l-CONF-26 EC27A I-CONF-27A EC27C I-CONF-27C M-EX-02D M-EX-02B M-EX-18 M-EX-19 M-EX-20 M-EX-20 M-^-10 GC/Quad (SCAN) M-AN-1 GC/Quad (SCAN) M-AN-34B GC/Ttappe {MS2) M-AN-10 GOQuad (SCAN) M-AN-28 GOQuad (SIM) M-AN-29 GOQuad (SCAN) M-AN-30A GOQuad (SCAN) M-AN-30B GOQuad (SIM) M-AN-30A GOQuad (SCAN) Anabolisants (* ) SPE Anabolisants (* ) SPE i has seuil Anabolisants (*) SPE (sans hydroiyse) Anabolisants (*) SPE (sans hydroiyse) k bas seuil Anabolisants (*) Hexane Clenbuterol ECIOA ECIOE ECIOB ECIOF EC19 EC18D I-CONF-1 OA I-CONF-1 OE I-CONF-1 OB I-CONF-1 OF I-C0NF-I9D I-CONF-1 8D M-EX-04D M-EX-04D M-EX-04D M-EX-04D M-EX-14 M-EX-13B M-AN-1 1 M-AN-07B M-AN-11 M-AN-07B M-AN-11 GOQuad (SCAN) GC/Trappe (MS2) GOQuad (SCAN) GCA^rappe (MS2) GOQuad (SCAN) M-AN-20C I GC/Tiappe (MS3) US AD A 0071 ^^ LNDD kl ^^ ENREGISTREMENT (LISTEl Codification ; L-CONF-01 Date : 09/06/2006 2/3 C p g^C\ WE^'^'^ ^^S CONFIRMATIONS REALISEES AU LABORATOIRE Epimethendiol 1 7Epimethandienone 6bctaOHmethandicnone Meth>dtestosterone Ml>12 Epioxandrolone, Oxandrolone, Tiirinabol-M 3'OH Stanozolol ( SI=25ng/inL) Zeranol et Taleranol (q et g Zearalanol) i Quali 19Nor(SI=100nfi/mL) Qitali 19Nor(SI=25nfi/mL) StabUiti 19Nor Quanti 19Nor (SI=lQOos/niL) Quanti 19Nor(SI=2Sng/mL) Semi Quanti T/E p-Treabolone Anabolisants * LCMS Anaboiisants * LCMS Analyse C12/C13dcs metabolites de la testosterone Terbutalioe EC19C EC20 EC21B EC39B EC23A EC23B EC23C EC23D EC24D EC22 EC22A EC22B EC31 I-C0NF-19C I-CONF-20 I-C0NF-21B I-CONF-39B I-CONF-23A I-CONF-23B I-CONF-23E I-CONF-23C I-CONF-23D I-CONF-24D I-CONF-22 I-CONF-22A I-CONF-22B I-CONF-31 M-EX-04E M-EX-14E M-EX-13B M-EX-39 M-EX-14 M-EX-14 M-EX-14D M-EX-14 M-EX-14 M-EX-04B M-EX-17 M-EX-03D M-EX-03D Reproterol, Fenoterol M-EX-24 Ivi-EX-i3A M-AN-21E M-AN-Il M-AN-22B M-AN-39 M-AN-U M-AN-24B MAN25B M-AN-25 M-AN-25 M-AN-27 M-AN-23 M-AN-47 M-AN-47 Salbutamol Salbutamol en MS2 Quanti Salbutamol >50to£ EPO EC34 EC18B EC18E EC18G I-CONF-34 I-C0NF-18B I-C0NF-18E I-C0NF-18G M-EX-34 M-EX-13A M-EX-13A ESQ? I I-CONF-07 IffiS Honnones ^tidiques LH - p-hCG Triamterene EC30 I-CONF-30 M-EX-13A M-EX-lg/28B M-AN-52 M-AN-41 M-AN-19 GOTrappe(SCAN) GC/Quad(SCAN) GC/Triq)pe(MS2) HPLC/MS3 ESI OaOuad (SCAN! GC^rappe (MS2) GC/Quad (SCAN) GC/Quad (SIM) GC/Quad (SIM) GC/Quad (SIM) HPLC/MS2 APCI HPLC/MS2ESI HPLC/MS3 ESI M-AN-U M-AN-19 M-AN-59 M-AN-19C M-AN-43 GC/MS (SCAN) GC/Quad f SG AlSn GC/Quad (SCAN) GOOuad (SCAN) GC/Trappe (MS2) GC/Quad (SIM) Immnnoditeciion Diur6tiques * Diur^tiques * Thiazides Amiloride ECo6 EC40 EC28A EC28B EC36A EC33A I-CONF-06 I-CONF-40 I-CONF-28A I-CONF-28B I-CONF-36A I-CONF-33A ^^M2 Inchis dans M-AN-06 M-EX-40 M-EX-03C M-EX-03C M-EX-36 M-EX-02A MtAN-3S - M-AN-08 - M-AN-53 M-AN-40 M-AN-33 M-AN-33 M-AN-33 M-AN-46 GC/MS {S( InnuuoQuorescence qumtilative ' InwiuDochnmatogiaphie GC/Quad fSCAN) HFLC/MS2 ESI HPLC/MS3ESI HPLC/MS2 ESI HPLC/MS2 ESI USADA 0072 ^ -^ LNDD ENREGISTREMENT (LISTE) Codification : L-CONF-01 Date : 09/06/2006 3/3 •o? £C\W£H. ISTE DES CONFIRMATIONS REALISEES AU LABORATOIRE ^^^Hi^^^^HHIHHi^^^^^l^^^^HII^^HH^^^^HI Bxemestane EC37 I-CONF-37 M-EX-27 M-AN-U GOOuadfSCAN) Tamoxifeoe-M, Cloniiphftne-M EC35 I-CONF-35 M-EX-35 M-AN-U GaQiiari (SCAN) ^H^HHII^IHI BBH^I^lii ■■I^^^H i^^^Hi ^^^^■^H Glucocorticbides * EC32A I-CONF-32A M-EX-29 M-AN-45 * 1 HPLCflklS2ESI GlucocorticoTdes * EC32B I-CONF-32B M-EX-29 M-AN-45 HPLC/MS3 ESI • : Terme g^nfirique, pour connaltre le detail des molecules concem6es consulter I'instruction I-CONF- coirespondante CONFIDENTiEL Date de creation Motif Date diffusion A Creation du document. 29/09/2003 B Ajout colonne des Essais + Mises h jour (I-C0NF-19D, I-CONF- 190) 05/04/2004 C changement d'identification des essais de confirmation aiout des conf LC, IRMS, HES, immuno et EPO 27/09/2004 D Ajout de la confiimation qualitative rcproterol, fenotCTol Ajout de la confimation quali / semi quantitative de la morphine ( surveillance minist&re) Modification de certains modes operatoires d'analyses suite a la suppression du satum 2004 Ajout de la confinnation du CIomiphene-M et du Tamoxifene Aiout de la confinnation de I'alpha et beta trenbolone par LCMS3 14/02/2005 E Recodification des essais EC09, EC28, EC32, EC22 07/02/2006 F Ajout de la conf quaii GC/MS2 du Salbutamol Ajout de la Conf LC/MS3 pour les metabolites du ziaranalol Ajout de la conf CG /SM des fonnes L et D de I'amphetamine et de la Methylamph^tamine Ajout de la confirmation g^n^rale en GC/MS2 des anabolisants 09/06/2006 USADA 0073 6^ LNDD MODE OPERATOIRE Codification : M-EX-04B Version : E Date :01/12/2005 1/3 METHODE DE PREPARATION - CONFIRMATION DE LA TESTOSTERONE ET DE L'EPITESTOSTERONE Documents cites : E-TE-03A, M-P-05, 1-EX-II, M-P-03B, I-TRAC-03A Attention : les temps d'hydrolyse et de derivation doiveDt imperativement etre respectfe. Remplir la fiche de preparation E-TE-03A r — ■ — - Designation Lavage k I'ether elapes en gris clair Hydrolyse itapes en trait epais Extraction - evaporation - derivation etapes en trait normal Blanc urinaire * * References * * Aliquote echantillon * * * Aliquote echantillon sans liydrolyse * Cq urinaire * Operations Prise d'essai = 2 mL Ajouter50tiLdeSI Materiel Tubeavis (13*100) Pipette Biohit l-5inL, cone Dispensette Rolling Centrifiigeuse 4000tr/min Pipette Pasteur Poire de prelevement Bain a sec Becher Reactifs et produits Diethylether (S06) APPLICABLF le [oi DEC. 2005] COHFlDFt^jl[l SPECI^AEN Azote ASSURANCE QUAUie LNDD Tube echantillon Gilson (12.5*100) Pipette Biohit l-5mL, cone Pipette a poussee positive Cone eppendorf 1 7aMethyItestosterone (SD-) a 4mg/L USADA 0074 ^5^ LNDD MODE OPERATOIRE Codification : M-EX-04B Version : E Date :01/12/2005 2/3 METHODE DE PREPARATION - CONFIRMATION DE LA TESTOSTERONE ET DE L'EPITESTOSTERONE Ajouter la (ou les ) substance{s) recliercheeCs) dans ie test de performance et les references Ajuster a pH =7 Ajouter I mL de tampon pH = 6.5 Agiter Ajouter une goutte de betaglu dans 1' aliquote echantillon a hydrolyser I Boucher et agiter 1 sec | I Hydrolyser 60 min a 55°C 1 Etuve Centrifiiger 5 min Exttaire sur SPE GILSON selonI-EX-11 (application anabo) Transvaser les eluats Evaporer environ 30 min Deriver en tube ferme 20 min a 6Q°C avec SQ^iL de reactif H Conditionner en vial plastique prealablement identifies selon I- TRAC-03A Pipette a poussee positive C5ne eppendorf Papier pH 0-14 Vortex Pipette Biohit l-5niL, cone Vortex Compte gouttes Vortex Centrifugeuse 4000tr/min Gilson Cartouche SPE CI 8 Tube recueil Gilson (12.5* 100) Tube avis (13*100) Bain a sec a 60°C, soufflettes Bain k sec a 60°C Seringue Hamilton lOOjiL Vial plastique SPECIMEN Flacon compte gouttes K2C03etCH3COOH Tampon pH=6.5 k -^"C (cfM-P-05) betaglucuronidase a +4°C ( b-glu) ''''^Nr/ti Azote Reactif H2 (cf M-P- 03B) USADA 0075 & LNDD MODE OPERATOIRE Codification : M-EX-04B Version : E Date :01/12/2005 3/3 METHODE DE PREPARATION - CONHRMATION DE LA TESTOSTERONE ET DE L'EPITESTOSTERONE Action : V Personhe coDcemee fiatte Signature " ,_ ^^ ^ redige par Esther CERPOLM 30/11/2005 ^^^^ verifie par Nathalie MECHIN 30/11/2005 ^^.^d^^^C- verifie par Aurehe LAURENT y\ \\.'^ — ' y . ■ 01/12/2005 C •^ < ^^>'Kfe Extraction Stockage Evaporation ?^(riobJl=^^SlS OUtfte J&^X) j-r^-^ao J5^S>b e^hgy^ RrgQ Bain 4 sec n" : A-tf-0 ^ T (°C ): Jt^lS J^6 9^5-5 ^o% JtJ^2o D^rivatioo Evaporation Reprise Stockage i Codetanipon:n^V9Crto^- O^ Diu enzyme it^OaOb Diu enzyme i t^OOOtj fQ^ Eftive n° : '^ Dlu NH40H : P b Q\"\&cn _>ca«jj Ife^ Giisonn°: nr-TYrwalnoot, ^ qPq. ^r+g toaUiP 3b ,lt^95 Jd'S^ Nfl_ ra jva_ Lieu: Ban i sec n° :c }A g^fe^ i^tj ML DirivatioD 1 Bain ^ sec n" : Jo Mi c r o onde Gede-eu dlu du rfactif 1 :COc6oG Derivation 2 Bain A sec n" : Dlu r&ctif 2 : Bain 4 sec o° : Lieu : to. dlu : daK limite d'utilisalion Cet enreg^stremeni est ii archiver dans le dossier de cor^rmatlon USADA 0079 ^3 TOPLEVEL PARAMETERS ri L-l ri ri ! i ^ I 1- n Method Information For: D:\MSDCHEM\l\METH0DS\MAN27.M Method Sections To Run: (X) Save Copy of Method With Data ( ) Pre-Run Cmd/Macro (X) Data Acquisition {X) Data Analysis ( ) Post-Run Cmd/Macro = Method Comments: Quantification du rapport Testosterone /Epitestosterone MSD20 injection en split END OF TOPLEVEL PARAMETERS INSTRUMENT CONTROL PARAMETERS ' Sample Inlet: GC Injection Source: GC ALS ' Mass Spectrometer: Enabled 68 90 GC METHOD LJ u 160 'C (On) 0.00 min OVEN Initial temp: Initial time: Ramps : # Rate Final temp 1 4.00 255 2 30.00 300 3 0.0 (Off) Post temp : ' C Post time: 0.00 min Run time: 28 .00 min FRONT INLET (UNKNOWN) Mode: Split Initial temp: 280 'C (On) Pressure: 175.0 kPa (On) Split ratio: 12.1:1 Split flow: 11.7 mL/min Total flow: 15.2 mL/min Gas saver: Off Gas type: Helium COLUMN 1 Final time 0.00 2.75 Maximum temp: 325 'C Equilibration time: 0.50 rain BACK INLET {) COLUMN 2 Method: MAN27.M Men Jul 24 17:17:53 2006 Page : 1 US ADA 0080 "^ I Capillary Column Model Number: Agilent 19091Z-002 HP-1, 0.2mm * 25m * . Hum Max temperature: 350 'C Nominal length: 25.0 m Nominal diameter: 200.00 urn Nominal film thickness: O.ll urn Mode: constant pressure Pressure: 175.0 kPa Nominal initial flow: l.O mL/min Average velocity: 41 cm/sec Inlet: Front Inlet Outlet : MSD Outlet pressure: vacuum (not installed) FRONT DETECTOR {NO DET) SIGNAL 1 Data rate: 20 Hz Type: test plot Save Data: Off Zero: 0.0 (Off) Range i Fast Peaks: Off Attenuation: o BACK DETECTOR (NO DET) SIGNAL 2 Data rate: 20 Hz Type: test plot Save Data: Off Zero: 0.0 (Off) Range : Fast Peaks ; Off Attenuation : COLUMN COM? 1 (No Detectors Installed) THERMAL AUX 2 Use: MSD Transfer Line Heater Description : Interface Initial temp: 280 'C (On) Initial time: 0.00 min # Rate Pinal temp Final time 1 0.0 (Off) COLUMN COMP 2 (No Detectors Installed) POST RUN Post Time: 0.00 min TIME TABLE Time Specifier Parameter & Setpoint 7673 Injector Front Injector: Sample Washes Sample Pumps Injection Volume 2.0 microliters Syringe Size 10.0 microliters Postlnj Solvent A Washes 3 Postlnj Solvent B Hashes 3 Viscosity Delay seconds Plunger Speed Fast Prelnjection Dwei: 0.00 minutes Postlnjection Dwell 0.00 minutes Back Injector: No parameters specified MS ACQUISITION PARAMETERS Method: MAN2 7.M Men Jul 24 17:17:53 2006 Page : 2 US ADA 0081 General Information Tune File Acquistion Mode MS Information n _j Solvent Delay EM Absolute EM Offset Resulting EM Voltage [Sim Parameters] L] lj Uj r , lJ| Hi LJJ M LJ I I GROUP 1 Group ID Resolution Plot 1 Ion Ions/Dwell In Group [MS Zones] MS Quad MS Source : atune . u : SIM : 2.50 ram : False : 400 : 1752 9 1 Low 301.3 ( Mass, Dwell) { Mass, Dwell) ( Mass, Dwell] ( 209.3, ( 341.3, { 432.4, 50) { 301.3, 50) { 417.3, 50) ( 446.4, 50) { 327.3, 50) 50) ( 431.3, 50) 50) ( 522.5, 50) 150 C maximum 200 C 230 C maximum 250 C END OF MS ACQUISITION PARAMETERS END OF INSTRUMENT CONTROL PARAMETERS DATA ANALYSIS PARAMETERS Method Name: D:\MSDCHEM\1\METH0DS\MAN27.M Percent Report Settings Sort By: Signal Output Destination Screen: No Printer: Yes Method: MAN2 7.M Mon Jul 24 17:17:53 2006 Page : 3 USADA 0082 !2 C File: No Integration Events: Autolntegrate Generate Report During Run Method: Signal Correlation Window: 0.020 No Quantitative Report Settings Report Type: Summary Output Destination Screen: Yes Printer: No File: No Generate Report During Run Method: No Quantification T/E (3 points) Calibration Last Updated: Hon Jul 24 17:15:46 2006 Reference Window: 2.00 Minutes Non-Reference Window: 1.00 Minutes Correlation Window: 0.10 minutes Default Multiplier: 1.00 Default Sample Concentration: 0.00 Compound Information 1) 17methyltestosterone (ISTD TR) Ret. Time 20.94 min., Extract & Integrate from 20.44 to 21.44 min, Lvl ID Cone (ng/ml) Response 1 100.000 5915926 2 100.000 4981326 3 100.000 5130998 ISTD cone: Curve Fit : Linear 100. 000 ng/ml 2) epi testosterone ( ) Ret. Time 18.52 min., Extract & Integrate from 18.02 to 19.02 min. Lvl ID Cone (ng/ml) Response 1 5.000 234336 2 30.000 1211449 3 60.000 2929592 Curve Fit: Linear, forced through origin Method: MAN27.M Mon Jul 24 17:17:53 2006 Page : 4 USADA 0083 f=' r 1 i "1 n Sequence Name: D:\MSDCHEM\l\SEQUEKCE\2407.S Comment : Operator: 28 Data Path: D:\Msd20\juilO6\2407\ Pre-Seq Cmd: Post-Seq Cmd: Method Sections To Run (X) Full Method { ) Reprocessing Only On A Barcode Mismatch (X) Inject Anyway ( ) Don't Inject Line Type Sample Saitple Sample Sample Sample Sample Sample 8 Sample 9 Sample 10 Sample 11 Sample 12 1 2 3 4 5 6 7 Vial DataFile Method Sample Name 1 RO MAN27 itms 2 TPITE MAN27 tp te2 1 Rl MAN27 itms 3 BLUITE MAN27 blu te 4 17807474 MAK27 178/07 995474 te 1 R2 MAN27 itms 5 BLURITE HAN27 blute G REFITE MAN27 blu t30 e5 7 REF2TE MfiN27 blu tl80 e30 8 REF3TE MAH27 blu t360 e60 9 CQITE MAW27 cq te 001 Sequence v6riW«P*''*- ^etnarquw'" Last Modified: Mon Jul 24 11:20:55 2006 Paae : T USADA 0084 1^ r-' DATA ANALYSIS PARAMETERS J " Ti Method Name: D:\MSDCHEM\l\METHODS\MAN27.M r ' r 1 r; 4 r-. U Percent Report Settings Sort By: Signal Ciutput Destination Screen: No Printer: Yes File: No Integration Events: Autolntegrate Generate Report During Run Method: No Signal Correlation Window: 0.020 Qualitative Report Settings Peak Location of Unknown: Apex Library to Search Minimum Quality DEMO . L . n. Integration Events: Autolntegrate ''"'' Report Type : Summary I ll Output Destination Screen: No Printer: Yes Hi File : No L) f Generate Report During Run Method: No Quantitative Report Settings Report Type: Summary Hi Ll Output Destination ■ ■' Screen: Yes ! 1 Printer: No ; ij Pile: No . , Generate Report During Run Method: No I J Method: MAN27.M Men Jul 24 17:15:54 2006 PaQe : 1 USADA 0085 -^ Quantification T/E (3 points) Calibration Last Updated: Mon Jul 24 17:15:46 2006 Reference Window: 2.00 Minutes Non- Re fere nee Window: 1.00 Minutes Correlation Window: 0,10 minutes Default Multiplier: 1.00 Default Sample Concentration: 0.00 Compound Information 1) 17methyltestast^rone {ISTD TR) Ret. Time 20.94 min. , Extract & Integrate from 20.44 to 21.44 min. Signal Rel Resp. Pet. Unc.(rel) Integration Tgt 301.30 man27.e Lvl ID Cone (ng/ml) Response 1 100.000 5915926 2 100.000 4981326 3 100.000 5130999 Qualifier Peak Analysis ON ISTD cone : 100.000 ng/ml Curve Fit: Linear 2} epi testosterone ( ) Ret. Time 18.52 min., Extract & Integrate froni 18.02 to 19.02 min. Signal Rel Resp. Pet. Unc. (rel) Integration Tgt 432.40 man27.e Lvl ID Cone (ng/ml) Response 1 5.000 234336 2 30. 000 1211449'. 3 60.000 2929592- Qualifier Peak Analysis ON Curve Fit: Linear, forced through origin 3) testosterone { ) Ret. Time 19.32 rain., Extract & Integrate from 18.82 to 19.82 min. Signal Rel Resp. Pet, Unc . (rel) Integration Tgt 432.40 man27 .e Lvl ID Cone (ng/ml) Response 1 30,000 1557516 ' 2 180,000 7052377. 3 360.000 17023691^ Qualifier Peak Analysis ON Method: MAN27,M Mon Jul 24 17:15:54 2006 Paqe:2 USADA 0086 1.,' Curve Fit: Linear, forced through origin ■1 J r I ; L..] END OF DATA ANALYSIS PARAMETERS Mon Jul 24 17:15:54 2006 Ul U u lJ ri Oi uj Method: MAN2 7.M Men Jul 24 17:15:54 2006 Paqe : 3 USADA0087 m