n -^ 1-1 --> D r. ■r n D ■LJ n n u SECTION 2 TECHNICAL PART 2.4 Confirmation analysis by GC/C/IRMS 2.4.1 GC/MS analysis ■~\ u USADA0123 TOPLEVEL PARftMETERS _lethod information For: C ■. \MSDCHEM\l\METHODS\MAN_52 . M " sthod Sections To Bun: Save Copy of Method With Data MS-POP Pre-Run Cmd/Macro Instrument Control Pre-Run Cmd/Macro Data Analysis Pre-Run Cmd/Macro Data Acquisition Data ftnalysis f^STOP Post-Run Cmd/Macro Instrument Control Post-Run Cmd/Macro Data Analysis Post-Run Cmd/Macro dethod Comments ; " This is the default method ) ) ) ) X) X) ) ) END OF TOPLEVEL PARAMETERS INSTRUMENT CONTROL PARAMETERS 6890 GC METHOD OVEN >- Initial temp: , Initial time: LJ Ramps : 7 'C (On) 1.00 min Maximum temp: 325 "C Equilibration time: 0.50 min U # 1 2 3 Post Post Bate Final temp 30.00 270 10.00 300 . (Off) temp : 70 ' C time: . 00 min Final time 12 3 00 ,00 Run time: 25 . 67 min iJ r ! FRONT INLET { SPLIT/S PLITLESS ) Mode: Splitless Initial temp: 280 'C (On) Pressure: 145.0 kPa (On) Purge flow: 20.0 mL/min Purge time: 2.00 min Total flow: 25.4 mL/min Gas saver: Off Gas type: Helium BACK INLET (UNKNOWN) [}° 0.25 um LUMN 1 Capillary Column Model Number: Agilent _ 190 91s-433 Max temperature: 325 'C Nominal length: 30 . m Nominal diameter: 250.00 um Nominal film thickness: Mode: constant pressure Pressure: 145.0 kPa Nominal initial flow: 2.3 mL/min Average velocity: 56 cm/sec Inlet: Front Inlet Outlet: MSD Outlet pressure: vacuum COLUMN 2 (not installed) ethod: MAN_52.M Mon Jul 24 14:19:20 2006 Page : 1 USADA0124 ^>f3 ; ^ONT DETECTOR ( ) IIGNAL 1 Data rate : 20 Hz Type : test plot ■ Save Data: Off Zero: 0.0 (Off) ^.. Range : i j Fast Peaks : Off ■ ■ Attenuation: "OLUMN COMP 1 .\ (No Detectors Installed) 'fHERMAL RUX 2 Use: MSD Transfer Line Heater ' i Description: ■ i Initial temp: 300 'C (On) '-■' Initial time: 0.00 min # Rate Final temp Final time n 1 0.0 (Off) BACK DETECTOR 1) SIGNAL 2 Data rate: 20 Hz Type : test plot Save Data: Off Zero: 0.0 [Off) Range : Fast Pealcs : Off Attenuation: COLUMN COMP 2 (No Detectors Installed) POST RUN Post Time: 0.00 min ' |IME TABLE '-- Time Specifier Parameter fi Setpoint n Ui I ! "7673 Injector Front Injector: Sample Washes Sample Pnmps Injection Volume Syringe Size Postlnj Solvent A Washes Postlnj Solvent B Washes Viscosity Delay Plunger Speed Prelnjection Dwell Postlnjection Dwell Back Injector: lo parameters specified Column 1 Inventory Number : ? Column 2 Inventory Number : 3 1,0 microliters 10.0 microliters 3 3 3 seconds Fast . 00 minutes . 00 minutes MS ACQUISITION PARAMETERS \ Seneral information , Tune File dcquistion Mode atune . u Scan MS Information } Solvent Delay ' fcM Absolute '■ EM Offset Resulting EM Voltage ;■ j[Scan Parameters] """IjOw Mass ' Method: MAN 52 .M ,T 9 . 00 mm False IBll. 8 50.0 Hon Jul 24 14:19:20 2006 Page : 2 USADA0125 yr^it ■ igh Mass ', hceshold Sample # ^51 ot, 2 low mass ' lot 2 high mass [MSZones] !~ B Quad " S Source 550.0 150 2 50 .0 550 . fi/D Samples 150 C maximum 200 C 230 C maximum 250 C END OF MS ACQUISITION PARAMETERS END OF INSTRUMENT CONTROL PftRRMETERS [I DRTA ANALYSTS PARAMETERS Method Name: C: \MSDCHEMVl\METHODS\MAN_52 . M Percent Report Settings I j Wort By: Signal ''lutput Destination ■ ; Screen: No L,! Printer: Yes File: No ni ■ integration Events: Autolntegrate i— 1- Generate Report During Bun Method: ] ignal Correlation Window: 0.020 No ' iualitative Report Settings W Peak Location of Unknown: Apex i ^library to Search 'c: \tempMRMS .L Minimum Quality 90 ■integration Events: Autolntegrate U' Report Type : Summary Output Destination Screen: No Printer: Yes File: No generate Repor t During Run Method: No Buantitative Report Settings Method: MAN 52. M Mon Jul 21 14:19:20 2006 Page : 3 USADA0126 445 ., sport Type: Summary [-Output Destination I ' Screen : Yes !._. Printer: No File: No ■ enerate Report During Run Method: No , alibration Last Updated; eference window: 10.00 Percent '■■ on-Ref erence window : 5.00 Percent 'iorrelation Window: 0,02 minutes Default Multiplier: 1,00 f efault Sample Concentration: 0.00 J:ompound Information '"-•*■* Empty Quantitation Database END OF DATA ANALYSIS PARAMETERS u Hon Jul 2i 14:19:20 2006 r n i n I ! n 1 1 I.-, n u ; Method: MAN_52.M Mon Jul 24 14:19:20 2006 Page : 4 USADA0127 ^^^ ' dditional Information for STERIFS.M , ile created Fri Mar 05 17:08:58 20D4 lethod : C: \MSDChemM\METHODS\DEFAULT .M ^ snamed: C: \MSDCHEM\l\METHODS\STERlFS -M ri Mar 05 17:08:58 2004 ] ethod : C:\MSDCHEM\l\METHODS\STERlFS.M ■ enamed: C:\WSDCHEMM\METHODS\STER1FSKETO.M >ue Apr 20 14:52:43 2004 iT ethod : C:\MSDCHEM\l\METHODS\STERlFS.M 'Unamed: C: \MSDCHEM\l\METHODS\MAN_52 .M Hed Nov 09 18:43:55 2005 r" Ui ■ I i-V n ethod: MAN 52 . M Mon Jul 24 14:19:20 2006 Page; 5 USADA 0128 ^^1 Sequence Name : C: \MSDChemM\5equence\200 6\ Juil0 6\23 07 , s ] Comment : Operator ; 4 9 Data Path: D:\MSD22\JUIL06\2307\ "".Top Pre-Seq Cmd : Instrument Control Pre-Seq Cmd : "Data Analysis Pre-Seq Cmd: Top Post-Seq Cmd: Instrument Control Post-Seq Cmd : 'Data Analysis Post-Seq Cmd: Method Sections To Run (X) Full Method ( ) Reprocessing Only On R Barcode Mismatch (X) Inject Anyway ( ) Don't Inject L.. Line 1) Calibration Data file Method 2) Blank 3) Sample Dataf ile Method Blank Sample Dataf ile Method Blank 7 ) Sample Dataf ile Method 8 ) Sample Dataf ile Method Sample Name/Misc Info 4) 51 6) 6 7 2307MixAc01 MAN_52 blulF3 MAN_52 17807'n4F3 MAN_52 blulFl MAN_52 n807-574Fl MAN_5 2 blulF2 MRN_52 17807474 F2 MAN_52 17807474F2b MAN 5 2 Blu 1 F3 Blu 1 Fl Blu 1 F2 Ui r- sequence virififc par : ^.H^-^i Remarques : ' ■ -V^ [_; Last Modified: Sun aul 23 10:17:10 2006 Page : 1 USADA0129 ■4-iS D:UMsd22Uuil06l2307\230TUtxActl1.D ' I i.-i n ! I U U! Li n Data File Name 2307MixAc01.D Data File Path D;\Msd22Uuil06\2307\ Operator 49 Date Acquired 7/23/2006 10:19 Acq. Method File MAN_52.M Sample Name Mix Ac 50 Vial Number 1 Misc Info Mix Acetate OOT 50 ng injects Temps de retention, temps de retention relatif et target Signal (M1 1 Name SaAndrostanoi AC RRt Time 10.69 Rel Ret Time Taraet Sianal 256 TarnRt Response 10,892,705 Etiocholanolone AC 14.35 1.343 272 20,821,485 Androsterone AC 14.62 1.367 272 35,520,111 5b Androstan 3a 17b diol diAC 15.17 1.419 256 20,304,691 5a Androstan 3a 17b diol diAC 15.57 1.456 316 28,264,859 11 KetoEtiocholanolone AC 17,07 1,597 271 27,735.914 Sb Prfionan 3a POM diol diAC 1920 1796 284 gfiB75 886 M2 signal Name 5a Androstanol AC Etiocholanolone AC Androsterone AC 5b Androstan 3a 17b dioi diAC 5a Androstan 3a 17b diol diAC 1 1 KetoEtiocholanolone AC ^i} Preana p ^i ?0a riini diAC Q1 signal Q1 Resn nnse Q1 Ratio 243 257 257 316 241 191 _22L 11,496,221 13,275,551 15,144,189 13.349.659 16,541,690 23,029,104 ^0053.051 105.5 63.8 42.6 90.4 58.5 83.0 56.3 n I ■ LJ M3 signal Name 5a Androstanol AC Etiocholanolone AC Androsterone AC 5b Androstan 3a 17b diol diAC Sa Androstan 3a 17b diol diAC 11 KetoEtiocholanolone AC ^b Pregna p ^a ?na diol diAC Page 1 of 2 204 201 218 241 256 286 344 O? sLonal n? Response QS-BaM 6,139.162 7,984,811 10,868,162 15,646,481 13,817,358 16,604,214 9.962.084 56.4 38.3 30.6 77.1 48.9 59.9 2^JL C:\MSDCHEM\CUSTRPT\MAN52.CRT 7^3/2006 11:33 AM US ADA 0130 -i^^ D:lMsd22Uull06l23OT\23OTMixAcO1.D r--. i... n i v.. n r", r-i : I r. u^ 5a Androstanol AC Etiocholanolone AC Androsterone AC 1.1 Li ri 1-; 5b Androstan 3a 17bdioldiAC 5a Androstan 3a 17b diol diAC u. 11 KetoEtiocholanolone AC 5b Pregnan 3a 20a diol diAC ™ i^^mm^mm^^ .M*H j \ / //i p\ L Page 2 of 2 C:\MS DCHEM\CUSTRP'nMAN52.CRT 7/23/200S11;33AM USADA0131 -fSo D:\MBd22Uull06\230T\blu1 F1 .D Data File Name blulFI.D Data File Path D:\Msd22\Jull06\2307\ Operator 49 Date Acquired 7/23/2005 12:10 Acq. Method File MAN_52.M Sample Name Blu 1 F1 Viai Number 4 Misc Info Blanc urinaire 1 Pool 4 Fraction 1 dans lOOpL i ! L,l L I ( I — I n r ] I I p. ■-V i t ^^°™~ 1 . L Temps tie retention, temps de retention relatif et target Signal (Ml) Name Rpt Time RftI Ret Time Tsrnfit Rianal Taraet ResDonse 5a Androstanol AC 10.68 258 5,234,507 Etiocholanolone AC 0,00 0,000 272 Androsterone AC 0,00 0.000 272 5b Androstan 3a 17b diol diAC 0.00 0.000 256 5a Androstan 3a 17b diol diAC 0.00 0,000 316 1 1 KetoEtlocholanolone AC 17,04 1.596 271 23,056,534 ^h Prpnnsn Ha ?0n riini diAC 0,00 ficino 284 n M2 signai Name ni sicinal 01 ResDonse 01 Ratio 5a Androstanol AC 243 5,447,955 104.1 Etiocholanolone AC 257 0,0 Androsterone AC 257 0.0 5b Androstan 3a 17b diol diAC 316 0.0 5a Androstan 3a 17b diol diAC 241 0.0 1 1 KetoEtlocholanolone AC 191 19,045,346 82,6 fih Prfionan 3a 20a diol diAC ?fi9 0,0 1 n ^j M3 signal Name O? sinnal 02 ResDonse 02 Ratio 5a Androstanol AC 204 2,943,791 56.2 Etiocholanolone AC 201 0.0 Androsterone AC 218 0,0 5b Androstan 3a 17b diol diAC 241 o.c 5a Androstan 3a 17b diol diAC 256 0.0 11 KetoEtlocholanolone AC Sh Preanan 3a 20a diol diAC 286 344 13,914,444 60.3 0.0 Page 1 of 2 C:\MSDCHEM\CUSTRPT\MAN52.CRT 7/23/2006 12:55 PM USADA 0132 -/^^ D:\M8d22UullOSU307U)lu1F1.D Ti I r" L n Etiocholanolone AC 5a Androstanol AC Androsterone AC n u I : i i L Sb Andro stan 3a 17b diol diAC 6a Androstan 3a 17b diol dIAC 11 KetoEtlocholanolone AC 5b Preqnan 3a 20a diol dIAC Page 2 of 2 C:\MSDCHEMVCUSTRPT\MAN52.CRT 7/23/2006 12:55 PM USADA0133 ^sa n ] j n i-.J r- I i U n u n ri D:Wlsd22UuilD6\230T\1790r4T4F1 .D Data File Name 17807474F1.D Data File Path D:\Msd22\Juil06\2307\ Operator 49 Date Acquired 7/23/2006 12:42 Acq, Method File MAN_52.M Sample Name 178/07 995474 F1 Vial Number 5 Misc Info 178/07 995474 Fraction 1 dans lOO^L Temps de retention, temps de retention relatif et target Signal (M11 Name 5a Androstanol AC RRt Time 10.69 Rel Ret Time Target Signal 258 Target Response 2,672,512 Etiochoianoione AC 0,00 0.000 272 Androsterone AC 0.00 0,000 272 5b Androstan 3a 17b diol dlAC 0.00 0.000 256 5a Androstan 3a 17b diol dlAC 0.00 0.000 316 11 KetoEtiocholanolone AC Sb Preanan 3a 20a diol diAC 17.05 noo 1.596 flOOO 271 ?fl4 27,520,882 M2 signal Name 5a Androstanol AC Etiocholanolone AC Androsterone AC 5b Androstan 3a 17b diol diAC 5a Androstan 3a 17b diol diAC 1 1 KetoEtioctioianolone AC 5h Pregnan 3a 2Qa diol diAC "1 siana' Q1 Response Q1 R^ti? 243 257 257 316 241 191 2,977,015 22.323,512 2 111.4 0.0 0.0 0.0 0.0 81.1 0,P M3 signal L.J I u u Name 07 sianal 02 Resoonse Q2 Ratio- 5a Androstanol AC 204 1,719,112 64,3 Etiocholanolone AC 201 0.0 Androsterone AC 218 0.0 5b Androstan 3a 17b diol diAC 241 0.0 5a Andnjstan 3a 17b diol diAC 256 0.0 1 1 KetoEtiocholanolone AC 286 16,694,242 60.7 fih PrRnnan 3a 20a diol diAC 344 0.0 I u Page 1 of Z C :\MSDCH EMVCUSTRPT\MAN52.CRT 7(23/2006 1:14 PM USADA0134 -^<33 D:\MsdZ2\Juil06\2307H T807474F1.D n' ] ; n 5a Androstanol AC srJ5«'|K]B;iEr,s*SrS :??n?2:=ri Etiocholanolone AC r' n ] ■ 5b Androstan 3a 17bdioldiAC Androsterone AC ^ =:i°'gi5=T™=E;H' T 3!;!=!ri = I = ^^j\j w y./\ f^J\^/'SC ^ s^^^sw*^^ ^-S:^ r—r-iOr'--^.^- JCs- 5a Androstan 3a 17b dioldiAC E= l=K:Sre=!r,= 5^^ n.r^e=l? l^.,H^v^'^^Mv.>^y^ = !r*:\Mid:iUuil06\23a7\178074T4F2b.D I : \ I L.J Data File Name 17B07474F2b.D Data File Path D:\Msd22\Juil06\2307\ Operator 49 Date Acquired 7/23/2006 14:33 Acq. Method File MAN„52.M Sample Name 178/07 995474 F2 Viai Number 7 Misc Info 178/07 995474 Fraction 2 dans 400mL D ri Temps de retention, temps de retention relatif et target Signal (M1) ! 1 1-;-' ri LJ U Name Rfit Time RelRptTime Tarciftt Sinnal Taroet Resoonse 5a Androstanol AC 10.69 256 6,790,329 Etiochoianolone AC 14,38 1.345 272 30,616,404 Androsterone AC 14.65 1.370 272 44,803,237 5b Androstan 3a 17b diol dlAC 0.00 0.000 256 5a Androstan 3a 1 7b diol dlAC 0.00 0.000 316 1 1 KetoEtiocholanolone AC 0.00 0.000 271 Sh Prpnnan 3a 20a diol diAC 00 0,000 284 M2 signal Name 01 signal 01 Response 01 Ratio 5a Androstanol AC 243 7,142,048 105.2 Etiochclanolone AC 257 19,396,055 63.4 Androsterone AC 257 19,255,218 43.0 5b Androstan 3a 17b dioi diAC 316 0.0 5a Androstan 3a 17b diol diAC 241 0.0 11 KetoEtiocholanolone AC 191 0.0 Sh Prptinan 3a 20a diol diAC 269 f> no M3 signal tviame 0? Rional 02 Resoonse O? Ratio 5a Androstanol AC 204 3,868,152 57.0 Etiochclanolone AC 201 11,568.610 37.8 Androsterone AC 218 13,516,338 30.2 5b Androstan 3a 17b diol diAC 241 0,0 5a Androstan 3a 17b diol diAC 256 0.0 11 KetoEtiocholanolone AC 286 0.0 .-^h Preanan 3a 2na diol diAC 344 0.0 .J Page 1 of 2 C:\HSDCHEM\CUSTRPT\MAN52.CRT 7/Z3/Z006 3:01 PM USADA 0138 -^^^ F=i n I . I,- D:\M*(J22Uun08\230TV1TB074T4F2b.D n r, u r u u hi p i. 5a Androstanol AC Etiocholanolone AC — ^11 , Androsterone AC 'iiim I 1 . — A f 1 / 5b Androstan 3a 17b diol dJAC 5a Androstan 3a 17b diol diAC n U n — / -■'"^ Jy' \ Sii:SiiHS:=i^^!i!!5:S=^1 — — J 1 / ™ J / / ,,„ 1 • w l. 11 KetoEtlocholanolone AC 5b Pregnan 3a 2Qa diol dIAC K' H^ "^^^'^^ '^:p€S^\T^^^C^^'^' iJ Page 2 of 2 C:\IWSDCHEM\CUSTRP-nMAN52.CRT 7/23/2006 3:01 PM US ADA 0139 A^l I, ' n n I n 1,1 n 1 ": 1-^ D:\M5dZZU uil06\23Dnl7807474F2.O Data File Name 17807474F2.D Data File Path D:\Msd22\Juil06\2307\ Operator 49 Date Acquired 7/23/2006 13:47 Acq. Method File MAN„52.M Sample Name 178/07 995474 F2 Vial Number 7 Misc Info 178/07 995474 Fraction 2 dans lOOtjL riiiiii ■MkX ^ 1 "^ II — ^ J 1 U'. J \j ; .A .. /VLmJJ J L Temps de retention, lemps de retention relatif et target Signal (Ml) Name 5a Androstanol AC RglTimg 10.69 Rel Ret Time Taroet Sianal 258 Taraet ResDonse 4,709,923 Etiocholanolone AC 14,56 1.365 272 169,848,822 Androsterone AC 14.84 1.388 272 213,976,918 5b Androstan 3a 17b diol dlAC 0.00 0.000 256 5a Androstan 3a 17b diol diAC 0.00 0.000 316 11 KetoEtiocholanolone AC 0.00 0.000 271 Sti Pretinan 3a ?0a diol diAC 0.00 nnoo 284 M2 signal Name 01 sinnal 01 ResDonse 01 Ratio 5a Androstanol AC 243 5,011,709 106.4 Etiocholanolone AC 257 104,358,276 61.4 Androsterone AC 257 91,230.541 42.6 5b Androstan 3a 17b diol diAC 316 0.0 5a Androstan 3a 17b diol diAC 241 0.0 1 1 KetoEtiocholanolone AC 191 0.0 ShPrfinnan 3a 70a diol diAC ?fi9 0.0 J J J M3 signal Narrip 0? sional n? RRsnnnae 07 Ratio 5a Androstanol AC 204 2,896,716 61,5 Etiocholanolone AC 201 59,514,197 35.0 Androsterone AC 218 61,028,102 28.5 5b Androstan 3a 17b dio! diAC 241 0.0 5a Androstan 3a 17b diol diAC 256 0.0 1 1 KetoEtiocholanolone AC 286 0,0 5h Preanan 3a 20a dio) diAC M4 0.0 Page 1 of Z C:\MSDCHEM\CUSTRPT\MANS2.CRT 7/23/2006 2:22 PM USADA 0140 -y^3 D:\MsdZ2Uull06\23a7\1T807474F2.D n fj u n n 1} lJ 5b Androstan 3a ITbdioldJAC 5a Androstanol AC — r==^^|S)5!WSiE«;^SI :;Si:'r=FI5 ■ •■M« '■■■■■ t nrriai.f . U A Etiocholanolone AC ::=n „..,.^,^ " — ..— — — — -- ■ -— — ■-— 1 11 KetoEtiocholanolone AC Androsterone AC Sa Androstan 3a 17b dlol diAC — / J '..^.H..j I'-.WF-.— J.D — i i / 1 '— • ^J-'-^ i^w--— -^ v^ _,i -"'^ "^ y' .... ,.- .... .... ..- .... ...- -." ■ •H ««« 5b Pregnan 3a 20a diol diAC v-'t^— :^"-'X''r.r^^::i — -_ - Page Z of 2 C:\MSDCH EM\CUSTRP'nMAN52.CRT 7/23/ZCX)6 Z;22 PM USADA0141 ^30 n I i n L. ■ r^ I '■ I , 1 lJ r"! u ■-. ri L, I I Lj a D:VMsil2:Uull06\23DT\blu1F3.D Data File Name blu1F3.D Data File Path D:\Msd22\Juil06\2307\ Operator 49 Date Acquired 7/23/2006 1 1 :00 Acq. Method File MAN_52.M Sample Name Blu 1 F3 Vial Number 2 Misc Info Blanc urinaire 1 Pool 4 Fraction 3 dans ^00\A. Temps de retention, temps de retention felatjf et target Signal (M11 tMD£ 5a Andrcstanol AC Re' Time 10.68 Rel Ret Time Taroet Sianal 258 Tarnpl Response 3,476,361 Etiocholanolone AC 0.00 0,000 272 Andfosterone AC 0,00 0.000 272 5b Androstan 3a 17b diol diAC 15,17 1.420 256 15,597,241 5a Androstan 3a 17b diol diAC 15,51 1,452 316 6,215,670 1 1 KetoEtiocholanolone AC 0,00 0.000 271 5h Preonan 3a ?0a diol diAC 19,14 1792 284 1R 549 438 1VI2 signal Name 5a Androstanol AC Etiocholanolone AC Androsterone AC 5b Androstan 3a 17b diol diAC 5a Androstan 3a 17b diol diAC 11 KetoEtiocholanolone AC 5b Preanan 3a 203 diol diAC Q1 sianal 01 Response Q1 Ratio 243 257 257 316 241 191 .^2. 3,650,999 14.170,551 3,187.095 ^365.521 105.0 0.0 0.0 90.9 61.1 0.0 M3 signal JMiS. i il 5a Androstanol AC Etiocholanolone AC Andnasterone AC 5b Androstan 3a 17b diol diAC 5a Androstan 3a 17b diol diAC 11 KetoEtiocholanolone AC §b Preonan 3a 20a diol dlAG n? sianal Q2 Response Q2 RatJg 204 201 218 241 256 286 344 1.954,169 12,280.836 2,634,418 "508073 56.2 0,0 0.0 78.7 50,5 0,0 _2LL Page 1 of 2 C:\N1SDCHEM\CUSTRPT\MAN52.CRT 7/23/200611:30 AM US AD A 0142 -/3^ 1 1 D:Mstl2ZUul106\230TUilu1F3.D Sa Androstanol AC i ; 1-.. n ! n L, n I J . i a [J. Eti oc hoi a nolone AC 5b Androstan 3a 17b dioldJAC Androsterone AC 5a Androstan 3a 17b diol dlAC 11 KetoEtiocholanolone AC 5b Preanan 3a 20a diol diAC "ZZ =!i»:!S[B5.a=ss;=; =i:l;?F — n P\ Page 2 of 2 C:\MSDCHEM\CUSTRP'nMAN52.CRT 7/23/200611:30 AM US ADA 0143 >/3^ i r. r\ Q D:(Msd22Uull06\230T\1T907474F3.D Data File Name 17807474F3.D Data File Path D:\Msd22\JiJil06\2307\ Operator 49 Date Acquired 7/23/2006 11:33 Acq. Method File MAN_52.M Sample Name 178/07 995474 F3 Vial Number 3 Misc Info 178/07 995474 Fraction 3 dans 400tJL JC153pt3"— 7T— — ~ 1 itJOOOCi t OOCOQ -kAL IW- — *^ U.J l^ -I a.OO nrr-- — *- Temps de retention, temos de retention reia tif et target Sipnat (M1 ) Name 5a Androstanol AC Ret Time 10.67 RpI Rfit Time Taraet Siana) 258 Taraet ResDonse 2,492,729 Etioctiolanotone AC 0,00 0.000 272 Androsterone AC 0-00 0.000 272 5b Androstan 3a 17b diol dlAC 15.10 1.415 256 3,658,105 5a Androstan 3a 17b diol diAC 15.48 1,450 316 1,968,201 11 KetoEtiocholanolone AC 0.00 0.000 271 fih Prsanan 3a 20a diol diAC 19.06 17R6 ?.R4 4flS1688 1 M2 signal Name 5a Androstanol AC Etioch Ola nolo ne AC Androsterone AC 5b Androstan 3a 17b diol dlAC 5a Androstan 3a 17fa diol diAC 1 1 KetoEtiocholanolone AC fihPrfignan3p?na dial diAC Q1 signal Q1 Respo nse Q1 Ratio 243 257 257 316 241 191 2,615,044 3,242,469 1,199,926 ^833947 104.9 0.0 0.0 88.6 61.0 0.0 M3 signal Name 5a Androstanol AC Etiocholanolone AC Androstensne AC 5b Androstan 3a 17b diot diAC 5a Androstan 3a 17b diol diAC 11 KetoEtiocholanolone AG Sh Preonan 3a ?0a diol diAC n? signal 02 Response QZBsHS. 204 201 218 241 256 286 344 1,395,444 2,877,543 985,712 1343.347 56.0 0.0 0.0 78.7 50.1 0,0 2L1 Page 1 of 2 C :\MS DCHEM\CUSTRPT\MAN52.CRT 7/23/2006 12:00 PM USADA0144 -Y33 r-i D:WI»(l22UuH0S\2307\17BO7474F3.D n. n [} D n I I ■-. n Li 1 1 u Lj Li IJ G iJl 5a Androstanol AC Etiocholanolone AC i^mj^re^pijE^i^^ T^Ttj^s %;r^^'^lM^'g'^^!tf':?2"'X- !!^^^?t^:^ Sb Androstan 3a 17b diol diAC — ^fnx^^ ■iISiiSfSB IWRJEBTR ?■ '"— " h rr: A ^ / A /\._ 11 Keto Etiocholanolone AC Androsterone AC 5a Androstan 3a 17b diol diAC 5b Pregnan 3a 20a diol diAC E;iE?e!te=?-ffiS "ffKSf!* .^ M r^_ 1 \ - m^^ f ,. J .— / 4 ^M. hr\\ "E Page 2 of 2 C:\MSDCHEM\CUSTRPT\MAN52.CRT 7/23/2006 12:00 PM US AD A 0145 -^3(< LNDD ENRBGISTEIEMENT Codification: E-CC-11 Version; B Date; 08/03/2006 1/1 VERIFICATION DES PERFORMANCES INSTRUMENTALES EN CG/SM (screening et confirmation) u. n ! . r>' u n Lj n U Numdro d'identification de Tappareil : t\Si> «iJ 3% RepeUer<35 Polaris Ion time > 2 ms Oui Non « pc u Observations : -. " , 2 - Etanch£Ite da svstfeme MSD 18/69 ( H20), 28/69 CN2), 32/69.(02), 44/69 (002) < 10% Polaris Air et ettn : Intensity ion 19 < intensity ion Observations : 3 -Sensibility Screening Recal / Mix confonne Conf TP confonne - Fichiw : i a o> t\;«. Kc o i ii" conionne - t'ictiier : 1 Jr* cooionne - tichier : TP confonne - Fichler: TP confonne - Fichier: Oui Non oi Oui Non (^ " 1 1 Observations : Code op6Bteur et paraphe : (^ «^ L- Cet enregistrement est a archiver dans h classew C-MA-Ech de Vappareil US AD A 0146 ^35 5973 Rutotune •N -, ^ r I: •N l- ■> — ■-, L-. r- u y Q J Sun Jul 23 10:11;55 2006 C:\MSDCHEM\1\597 3N\RTUNE.U Instrument: MSD22 Mass Pw50 69.00 421715 0. SI 66 IL Mass 219.00 Ab 437153 Pw50 0.61 Mass 502.00 Ab 54028 Pw50 0.62 71 — T — •- 216 Y\ Ion Pol POS MassGain 267 MassOffs -10 Emission 34.6 AmuGain 2179 ElEnirgy 69.9 AmuOffs 130 Filament 2 Wid219 -0.037 ■ DC Pol NEG Repeller 21 . 26 lonFcus 90.2 HEDEnab EntLens 21.0 EMVolts EntOf fs 17 . 57 Zones : MS Source MS Quad 230 Foreline 150 221 500 505 Scan: 10.00 - 700.00 Samples: 8 Thresh; lOO step: 0.10 119 peaks Base: 219.00 Abundance: 389440 100 -I 90 - 80 - 70 ■ 60 - 50 ■ 40 - 30 - 20 - 10 - ,^^-v-^ 100 200 300 400 500 600 Mass Abund Rel Abund Iso Mass Iso Abund Iso Ratio 373184 100.00 70.00 4003 1-07 389440 104. 36 220.00 17152 4.40 50000 13.40 503.00 5043 10. 09 69. 00 219. 00 502. 00 ON 1812 Samples 8 PFTBA OPEN Averages 3 Stepsize . 10 93 USADA 0147 ^3^ \ I 5973 Air and Water Check F^ n Instrument: MSD22 Sun Jul 23 10:12:58 2006 C:SMSDCHEMM\5 9 73N\ n Li' U n n Q '] I i Lj u Scan: 10 69 peaks 00 - 75 Base : .00 Samples: 8 Thresh: Step: 69 . 00 Abundance : 322 304 . 10 100- 95- 90- 65- BO- 75- 70 - 65- 60- 55- 50- 45- 40- 35- " 30 ■ ■- - — — ■ ■ — ^..— _ — ■ 7 25 ■ 20 - 15 - 10 - 5 - 1 J 1 1 .^ 1 - 1 ■"T" ' > 1 1 1 1 1 |— H 1 1 1 1 1 1 1 1 1 >— ■ r 1 1 1 1 10 20 30 40 50 60 70 Mas E 69.00 18.10 28. 00 Abund Rel Abund Iso Mass Iso 322304 100.00 70.00 3336 1.04 19-00 3013 0.93 28.90 Abund Iso 3612 34 58 Ratio 1. 12 1. 02 1. 92 Current Pa rams used: ATUNE . U Relative abundances : y 16/69 1= 1 04 Water% 28/69 = 93 Nit rogen% 32/69 = 23 Oxygen% 44/69 — 17 Carbon Dioxide* 28/18 = 90 32 Nitrogen/Water% y USADA0148 v/3^ LNDD ENREGISTREMENT CodificatiDn : Version : Date: E-FCR-09 A 31/01/2006 1/3 FiCHE D'ANALYSE / RESULT AT ANALYSE QUALITATIVE GC/MS POUR CONFIRMATION GC/CARMS i r\ Echantillon : 178/07 995474 r L.. Tolerances fix6es par I'AMA { document : WADA Technical Document - TD2003IDCR ) Tolerances sur le tr et le Ht : +/-1% ou +/- 0,2 min (prendre la plus faible des deux) Pour les ^ondances relatives > 50% il est admss +/- 10% (en absolu ) de variation 25 i I '■ r-. LNDD ENREGISTREMENT Codification : E-FCR-09 Version : A Date : 31/01/2006 2/3 FICHE D'ANALYSE / BESULTAT ANALYSE QUALITATIVE GC/MS POUR CONFIRMATION GC/C/IRMS I r: u D Substance caract^risfie : Androst^rone AC Fichier : 17807474F2b Concordance des Tr : oui Concordance des Trr : oui Concordance globale des abondances relatives : oui X non non nan X X Ui r: u Substance caractSrisee : 5b Androstane-3a,17b-diol diAC Fichier ; 17807474F3 Mix Echantillon Tr(niin) In- Ml (%) M2 (%■> M3 (%) TrCmin) Trr 1 Ml (%) M2 (%) M3(%) 15.17 1.419 100 90.4 77.1 15.1 1.415 1 too 88.6 78.7 Tolerance basse 15.02 1.405 80,4 67.1 - : Tolerance haute 15.32 i.433 100,4 87.1 _,- .. Concordance des Tr : ou' Concordance des Trr ; oui Concordance globale des abondances relatives : oui X non non non X X Substance caractfiris^e : 5aAndrostane-3a,l7b-diol diAC Tolerance basse Tolerance haute Mix Tr (mill) 15.57 I5.41 15.73 Trr 1.456 1.441 1.471 Fichier : I7807474F3 M2 (%) 58.5 48.5 68.5 M3 (%) 48.9 39.12 58.68 Echantillon Tr(min) 15.48 Trr 1.450 Ml (%) 100 M2 (%] 61 M3 (%) 50.1 Concordance des Tr : Concordance des Trr : Concordance globale des tendances relatives : oui oui oui X non non non X X Substance caracterisSe : | 5b Pragnane-3a.20a-d]ordLAC Fichier : 17807474F3 Echantillon Ml (%) 100 M2 (%) 57.2 Concordance des Tr : Concordance des Trr : Concordance globale des abondances relatives : OUI oui oui X noD non non X X USADA0150 ^3^ K- F-. Codification : E-FCR-09 LNDD ENREGISTREMENT Version : A Date : 31/01/2006 3/3 FICHE D' ANALYSE / RESULTAT ANALYSE QUALITATIVE GC/MS POUR CONFIRMATION GC/C/IRMS n ; i I' Substance cara^t^ris^e : Fichier : Mix Ecbantillon Tr fmin) Tit Ml (%) M2(%) M3 (%) Tr(niin) Trr M] (%) M2 (%) M3 {%) 100 too Tolerance basse Tolerance haute Concordance des Tr : oui Concordance des Trr : oui Concordance globale des abondances relatives : out non non non rj i i I U Substance caract6ris6e : Fichier : .. -.... Mix Echantillon | h- Tr (min) Trr Ml(%) M2 (%) M3 (%) Tr(mtn) Tit Ml (%) M2 (%) M3 (%) 1 100 100 1 i Tolerance basse ■ . -,. Tolerance haute ■- Concordance des Tr : out oui oui non Concordance des Trr : non Concordance globaie des abondances relatives : non Paraphe et code opSraleur : "'^jI^ Partie 6 remplir par le responsable ; Caract6risatio]i formelle de tous les analytes : Paraphe et code opSrateur : OUI ^ non ■ Hq rjp> Observations ; Cel enregistrement est a archiver dans le dossier de confirmation de VechantiUon IJ USADA0151 A\^o