1...

LNDD

ENREGISTREMENT

Code:

Version :

Date:

E-RECAP-Ol
J

09/06/2006

FICHE RECAPITULATIVE DES ANALYSES PRESENTEES

Ess^ n° :

Mode operatoire de preparation :

Mode operatoire d'anaiyse :

CG/TSD I I CG/SM(SIM) | |

Concentration mesuree:
* Seuil corrige :

ES02 -BBS (CG-SM) [^
ES02C -EPH (CG/SM) 1
ES03-CD{CySM) 1^
ES04 -H (CG/SM) |^
ES03C-LCH(CL/SM)[^

ES08 -HES (CG/SM) [ |
ES08B -PS 1 I

ES06 - IMM
ES07 -EPO

ES03B -LCH (CL/SM/SM)[
ES05 -MS2 (CG/SM/SM)[

□

ESSOl - HBOCsl I
ESS02 - IS I 1

Code operateur de I'analyste /^O
Date et paraphe : ou{o%lo(,

Hors portee d'accreditation : | \

Raison ou numero d'ecart de la declaration en hors port^e :

Code operateur du responsable : l**
Date et par^he : £) u, / 0^ / OQ,

Cet enregistrement est a archiver dans le dossier de confirmation

* k remplir par le responsable US ADA 0260

331

LNDD

MODE OPERATOERE

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-H, M-P-03B, I-TRAC-03A

Attention : les temps d'hydrolyse et de derivation doivent imperativement etre respectes.
Remplir la fiche de preparation E-TE-03A

Designation

Lavage a I'ether
stapes en ^is clair

„„..., ■ — ,

Hydrolyse
e tapes en trait epais

Extraction - evaporation

- derivation
etapes en trait normal

Blanc urinaire

*

*

References

*

*

Aliquote echantillon

*

■k

*

Aliquote echantillon sans

hydrolyse

*

Cq urinaire

*

Operations

Materiel

Tube a vis (13*100)

Pipette Biohit l-5niL, cone

Dispensette
Rolling

Centrifugeuse 4000tr/min

Pipette Pasteur
Poire de prelevement

Reactifs et produits

Diethylether (S06)

APPLICAPi.li; '-

1 DEC. 2005

Pnse d'essai = 2 mL

Ajouter SOfiL de SI

Bain a sec

Becher

Azote

ASSURANCE Qb^LITE
LNDD

Tube echantillon Gilson (12.5*100)
Pipette Biohit l-5mL, cone

Pipette a poussee positive
Cone eppendorf

1 7aMethyltestosterone
(SI3-) a 4mg/L

USADA 0261

3^

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

Aj outer la (ou les ) sabstance(s)
recherchee(s) dans le test de
performance et les refeiences

Ajuster k pH =7

Ajouter ImLde tampon pH= 6.5

Pipette a poussee positive
C6ne eppendorf

?^ierpH0-14
Vortex

Pipette Biohit l-5mL, c6ne

Agiter

1 Ajouter line gouttedebetaglu dans 1' I
aliquote fehantillon Jt hydrolyser |

I Boucher et aRiter 1 sec |

Vortex

Compte gouttes

Vortex

I Hydrolyser60mina55°C 1 Etuve

Centrifugeuse 4000tr/niin

CeatrifiiRer 5 mm

Extraiie sur SPE GE^ON
selon I-EX-1 1 (application anabo)

Traosvaser les eluats

Evaporer environ 30 mip

Deliver en tube fermi
20 min a 60°C avec SOfxL de reactif H

i lj

Conditionner en vial plastique

prealablement identifies selon I-

TRAC-03A

Gilson

Cartouche SPE CIS

Tube recueU Gilson (12.5* 100)

Tube avis (13*100)

Bain a sec a 60°C, soufflettes

Bain k sec a 60''C
Seringue Hamilton 100|iL

Vial plastique

Flacon compte gouttes
K2C03 et CH3C00H

Tampon pH=6.5 k +4=C
(cfM-P-05)

beti^ucuronidase

+4°C(b-glu)

i^

Azote

Reacdf H2 (cf M-P-
03B)

USADA 0262

T>k

LNDD

MODE OPERATOIRE

Codification : M-EX-04B
Version : E
Date :01/12/2005

. 3/3

METHODE DE PREPARATION - CONFIRMATION DE LA TESTOSTERONE ET DE

L'EPITESTOSTERONE

Revision biennale +

- I'evaporation des phases organiques se fait maintenant sous azote (h-

INFO du 10/05/04)

aiout de I-CONF-24D et I-CONF-24E

10/09/2004

Suppression de I-CONF-24E

Ajout des consignes concemant Is eg urinaire

Ajout d'un synthese pour clarifier les differentes etapes que doit subir le
eg, le blanc urinaire Taliquote echantillon ...

18/04/2005

01/12/2005

r

SPECIMEN

USADA 0263

3S

J

lJ

LNDD

EXREGISTREMENT

Codification . E-TE-03A

Version : M

DaK : 13/09/2005

.THE BE sum PES AT .n.OTF.S POLRLA CONHBMAT.QN /COMRL EXPERT SE EN GC

EchamiUon :

■178/cl~ '^'^? 4^fr 1 Mode operatoire d'extraction ; M - £ V- 0^^

Date

oy^M-

oyaioi

Appareil

pHmet n° - ~¥

Refract n° 2-

Temperature en °C

2t£.

Valeur affichee

v^

A_.o^<

Parariie

^r"

Date de mise a L'ambiant de l' 6chantilloii|g^/ c^/;^^
Prise d'essai PE :

Heure de mise a i'ambiam ■. | 6 H -^ 2.

dlu : date limite tf utilisation

Cet enregislremeni est a archiver dam k dossier de confirmalion

USADA 0264

36

TOPLEVEL PARAMETERS

Method information For: D:\MSDCHEM\l\HETHODS\MRN27.M
Method Sections To Run:

CX) Save Copy of Method With Data

( ) Pre -Run Cmd/Macro =

{X) Data Acquisition

(X) Data Analysis

( ) Post-Run Cmd/Macro =

"luantS^Sion du rapport Testosterone /Epitestosterone MSD20 injection
en split

END OF TOPLEVEL PARAMETERS

INSTRUMENT CONTROL PARAMETERS

Sample Inlet:
Injection Source:
Mass Spectrometer:

GC

GC ALS

Enabled

68 90 GC METHOD

; I
1 I '

160 'C (On)
0.00 min

OVEN

Initial temp:
Initial time:
Ramps :

# Rate Final temp

1 4.00 255

2 30.00 300

3 O.O(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: 170.0 kPa (On)
Split ratio: 12.1:1
Split flow: 11.3 tnL/min
Total flow: 14.8 mL/min
Gas saver: Off
Gas type: Helium

Final time
0.00
2.75

COLUMN 1
Method: MAN2 7.M

Maximum temp: 325 'C
Equilibration time; 0.50 min

BACK INLET

COLUMN 2

Thu Aug 03 14:52:27 2006

Page : 1

USADA 0265

y

CaDillary Column

Sel Nu!rQ=er: Agilent 19091Z-002
HP-1, 0.2mm * 25in * O.llum
Max temperature: 350 'C
Nominal length: 25.0 m
Nominal diameter: 200.00 urn
Nominal film thickness: 0.11 um
Mode: constant pressure

Pressure: 170.0 kPa

Nominal initial flow: 9 mL/mm

Average velocity: 40 cm/sec

Inlet: Front Inlet

Outlet: MSD

Outlet pressure: vacuum

FRONT DETECTOR (NO DET)

SIGNAL 1

Data rate; 20 Hz
Type: test plot
Save Data: Off
Zero: 0.0 (Off)
Range :
Fast Peaks: Off
Attenuation:

COLUMN COM? 1 .-, jx

{No Detectors Installed)

THERMAL AUX 2

use: MSD Transfer Line Heater
Description: Interface
Initial temp: 280 'C (On)
Initial time: 0.00 min

# Rate Final temp Final time
1 o.O(Off)

{not installed)

BACK DETECTOR (NO DET)

SIGNAL 2

Data rate: 20 Hz
Type: test plot
Save Data: Off
Zero: 0.0 (Off)
Range:
Fast Peaks: Off
Attenuat ion :

COLUMN COMP 2

(No Detectors Installed)

POST RUN

Post Time :

0.00 min

TIME TABLE
Time

Specifier

Parameter fc Setpoint

7673 Injector

Front injector:
Sample Washes
Sample Pumps
Injection Volume
Syringe Size

Postlnj Solvent A Washes
postlnj Solvent B Washes
Viscosity Delay
Plunger Speed
Prelnjection Dwell
Postlnjection Dwell

Back Injector:
No parameters specified

2.0 microliters
10.0 microliters
3
3
seconds

Fast

0.00 minutes

0.00 minutes

MS ACQUISITION PARAMETERS

Method: MAN27.M

Thu Aug 03 14:52:27 2006

Page; 2 \^
USADA 0266

General Information

Tune File
Acquistion Mode

atune . u
SIM

MS Information

Solvent Delay •

2.50 min

EM Absolute =
EM Offset =
Resulting EM Voltage

False

400

1752.9

[Sim Parameters]

GROUP 1
Group ID
Resolution
Plot 1 Ion
Ions/Dwell In Group

: 1
: Low
: 301.3
( Mass,

Dwell) (

Mass,

( 209.3,

50) (

301.3,

C 341.3,

50) (

417.3,

-'

( 432.4,

50} {

446.4,

^- [MSZones]

i T. MS Quad
i ■ MS Source

: 150 C
: 230 C

maximum
maximum

200 C
250 C

50) ( 327.3, 50)
50) ( 431.3, 50)
50) ( 522.5, 50)

END OF MS ACQUISITION PARAMETERS
END OF INSTRUMENT CONTROL PARAMETERS

DATA ANALYSIS PARAMETERS

Method Name: D:\MSDCHEM\l\METHODS\MAN27.M

Percent Report Settings

Sort By: Signal

Output Destination
Screen: No
Printer: Yes

Method: HAN2 7.M

Thu Aug 03 14:52:27 2006

Page : 3
USADA 0267

3?

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

' Subration Last Updated: Thu Aug 03 09:24:50 2006

L..

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

Ret. Sf'2"9rSn°?°Extra=t . Integrate t.oJ'l7..?L 21.40 min.

Lvl ID

1

2

3

Cone (ng/mL)
100.000
100.000
100.000

Response
4741732
3738708
4816134

ISTD cone:
Curve Fit: Linear

100.000 ng/mL

Ret. ?Srir4rSn., Extract .integrate from 17.99 to 18.99 r„in.

Lvl ID

1

2

3

Cone (ng/mL) Response

5.000 129729

30.000 534747

50.000 1904191

^^ Curve Fit: Linear, forced through origin

Method: MAN27.M

Thu Aug 03 14:52:27 2006

Page:40
USADA 0268

"N

(■;

DATA AMALYSIS PARAMETERS
Method Name: D:\MSDCHEM\l\METHODS\MAN27.M

Percent Report Settings

Sort By: Signal

Output 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 °

Integration Events: Autolntegrate
" Report Type: Summary

; I Output Destination
Screen: No
Printer: Yes
File; No

, I

" Generate Report During Run Method: No

] I

1 I

^ Quantitative Report Settings

I I ^ " ^-- "■

] '

"■ Report Type: Summary

: i \ Output Destination
'^ Screen: Yes

Printer: No
, i , File: No

:"■' Generate Report During Run Method: No

■" Method: MAN27.M Fri Aug 04 07:32:57 2006 Page:

USADA 0269

^1

Quantification du rapport T/E 07:32:46 2006
Calibration Last Updated: Fri Aug U4

Reference Window: 2.00 Minutes
SSn-Reference Window: l. 00 Minutes
correlation Window: 0.10 minutes
Default Multiplier: 1.00
Default Satr¥.le-Cb>icentration: 0.00

Compound Information

(ISTD TR)
1) Methyltestosterone

,et Tin,e .0 . .1 .in. , Extract . Integrate fro™ 20.4Xto 21.41 .in.
RelResp. Pct. UnCrel, I-eff^-

Tgt 301.30

■ Lvl ID cone ing/mL) R^^ponse
T 100.000 3782021

. 2

"' 3

100.000
100. 000

3011193
3783290

Qualifier Peak Analysis ON ISTD cone;
Curve Fit: Linear

100.000 ng/niL

Epi testosterone

Ret. Time 18.50 mm

Signal Rel Resp . Pet. Unc.(rel)
Tgt 432.40

( )

Extract Sc Integrate from 18.00 to

19.00 min.

Integration
man27.e

Lvl ID Cone (ng/mL) Response

1 5.000 294592

5 30.000 1324358

i 60.000 3442296

Qualifier Peak Analysis ON
Curve Fit: Linear

'■ J

i I .

( TR)
3) Testosterone

.et.Tr.e 13 . 30 .in. , Extract . Integrate fro. 18.80 to 1..80.in.

Integration
man27 .e

Signal Rel Resp.~ Pet. Unc.(rel)
Tgt 432-40

Lvl ID Cone (ng/mL) Response

1 30.000 1845917

2 180.000 7860237

3 360.000 20557109

Qualifier Peak Analysis ON

Method: MAK27.M Fri Aug 04 07:32:57 2006

Page:£|2*

USADA 0270

Curve Fit : Linear

r-i

EHD OF DATA ANALYSIS PARAMETERS

Fri Aug 04 07:32:57 2006

Method: MAN2 7.M

Fri Aug 04 07:32:57 2006

Page : U%
USADA 0271

sequence Name: D-.\MSDCHEM\1\SEQUENCE\0308 .S

Comment ;

DSffaS; "\Msd20\aoutO6\0308\

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

Vial DataFile Method Sample Naine

1 Sample

2 Sample

3 Sample

4 Sample

5 Sample

6 Sample

7 Sample

8 Sample

9 Sample

10 Sample

11 Sample

12 Sample

13 Sample

14 Sample

1 Rl

2 TPTE

I R2

3 BLXJTE

4 1780774A

5 1780774B

6 1780774C

7 1780774S

1 R3

8 BLURTE

9 REFITE
10 REF2TE

II REF3TE
12 CQTE

MAN27

MAN27

MAN27

MAN27

MAN27

MAN27

MAN27

MAK27

MAH27

MAK27

MAN27

MAN27

MAN27

MAN27

itms

TP TE 2

itms

BLU TE

B 178/07 995474 TE

B 178/07 995474 TE

B 178/07 995474 TE

B 178/07 995474 ssh TE

itms

BLU TE

BbU + T3 E5

BLU + T180 E30

BLU + T360 E60

CQ TE 001

Sequence verifiee par : fe:.oX

Remarques ; .- "*

u.

Last Modified: Thu Aug 03 16:30:37 2006

Page: (ill

USADA 0272

L,..-

Response Ratio

5-

4-

Testosterone

L-.

!i

Amount Ratio

Resp Ratio = 1.50e+000 * Amt - 7.81e-003
Coef of Det (r"2) = 0.999 Curve Fit: Linear

I LJ

Method Namet D:\MSDCHEM\l\METHODS\MAN27.M

Calibration Table Last Updated: Fri Aug 04 07:32:46 2006

USADA 0273

kS

U'

Response Ratio

0.9-

0.8-

0.7-

0.6-

0.5-

0.4-

0.3-

0.2-

0.1-

Epi testosterone

0.2 0-4

Amount Ratio

0.6

Resp Ratio = l.Sle+OOO * Amt " 3.72e-003
Coef of Det (r-2) = 0.999 Curve Fit: Lmea

ar

S^SaS^^XaSirS^fS^^^^el^ - -^^- 0,..« .OOS

USADA 0274

46

File: D:\Msd2 0\aout06\0308\BLUTE.D

Operator: 23

Date Acquired: 3 Aug 2006 18:12

Instrument: MSD 20

Method File: MAN27

Sample Name: BLU TE

Misc Info:

Vial Number : 3

Analyse quantitative :Testosterone/Epitestosterone

r

SI :METHYLTESTOSTERONE

Abundance

eoooo

Ion 301 ,30 (301.00 to 302.00): BLUTE.D
2Cl92

60000

40000

21.51

-

20000

rm»->

I

1 1 J L 1 1 1 1 1 . I < I 1 .. I 1 1 1 1 1 1 1 1 1 1 1

20,50 21.00 21-50 22.00 22.50

Epitestosterone -Testosterone

Abundance

Ion 432.40 (432.10 to433.10): BLUTE.D

2ad

2000

16.62

1500

1000

1B.3B
1

/

500

-^

\j

19.53 (

1 1 > < 1 I I . 1 1 I . I 1 1 . . . < 1 1 1 . . 1 > 1 . 1 1
13.50 19,00 19.50 20.00 20.50

Epitesto-Testo-llbetaOH A et E

yjundance

Ion 432.40 {432.10 to 433.10): BLUTE.D

Ion 522.50 (522.20 to 523.20): BLUTE.D 2aj

2000

18.62

1500

1000

18.3^,

1

53

1

500

rime->

:^=A}^

19.53 (

■ ■ ■ ■ 1 ■ ■ ■ 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1

1B.50 19.00 19.50 20.00 20.50

1

page 1

k^

USADA 0275

File: D:\Msd20\aout06\03 08\BLURTE.D

Operator: 23

Date Acquired: 3 Aug 2006 21:18

Instrument: MSD 20

Method File: MAN27

Sample Name: BLU TE

Misc info:

Vial Number : 8

Analyse quantitative :Testosterone/Epitestosterone

SI :METHyLTESTOSTERONE

Sundance

150000

100000

50000

L

I ,

TIC: BLURTE.D

rime-> 5.O0 10.00 15.00 20.00

Bpitestosterone-Testosterone
Abundance Ion 432,40 (432.10 to433.10): BLURTE.D

2000

1500

1000

500

16.38

2CS

1B.62

rirrie->

Epitesto-Testo-llbetaOH A et E

yjundance lofi 432.40 (432.1 to 433.10): BLURTE.D

Ign 522.50 (522.20 to 523.20): BLURTE.D 2Ct9

18.50 19.00 19.50 20.00 20.50

page 1

it?

USADA 0276

File: D:\MSD20\AOUT06\0308\178 0774A.D

Operator: 23

Date Acquired: 3 Aug 2006 18:43

Instrument: MSD 2

Method File: MAN27

Sample Name: B 178/07 995474 TE

Misc Info:

Vial Number : 4

Analyse quantitative :Testosterone/Epitestosterone

SI :METHYLTESTOSTERONE

Abundance
2500000

TIC:1780774A.D

2000000

1500000

1000000

500000

i

JJ.iLa-aI

ii,MJU.AjLj_

,Au-u

J

L

JiA-oWi-'

nme~> 5.

DO 10.00 15.00

20,00

Abundance
120000

100000
80000

60000

400QO

20000

L

Ion 301.30 (301,0010 302,00); 17B077'1A,D
196

21,22

0,11

22,56

22-02

ime->

20-50 21.00 21,50 22-00 22.50

Epitestosterone-Testosterone

Ion 432.40(432-1010 433,10); 1780774A,D
1£l36

\bundance

100000

80000

60000

40000

20000

nme->

B,10

19.62

20.11

19.60

t /TYN

■-■-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

yjundance ion 432-40 (432,101o 433.10): 17e0774A,D

Ion 522.50 (522,20 to^p20); 1780774A,D

400000

300000

200000

100000

[Tlme->

19,80

lelsO 19-00 19.50 20.00 20,50

page 1

USADA 0277

D:\MSD20\AOUT06\030a\17B0774A.D

L-!

Data File Path

D:\MSD20\AOUT06\030S\

Data File Name

1780774A.D

Operator

23

Date Acquired

8/3/200618:43

Acq. Method File

MAN27

Sample Name

B 178/07 995474 IE

Vial Number

4

Calibration Title

Quantification du rapport T/E

Last Calibration Update

Fri Aug 04 07:32:46 2006

# PeakTvoe Ret Time

Siqnal Name

1) "ISTD 20.98

301 .3 Methyltestosteron

2) 18,56

432.4 Epitestosterone

3) " 19.36

432.4 Testosterone

Target Response Amount Units

3971127 100.00 ng/mL

342595 5.94 ng/mL

3733052 63.15 ng/mL

r:

Caicul du rapport T/E

Surface Concentration
10.9 10.6

Page 1 of 1

D:\MSDchem\Custrpt\MAN27.CRT

S/*2006 7;39 AM ^^

USADA 0278

D:\MSD20\AOUT06\0308\1T80T74B.D

' '

Data File Path

D:\MSD20\AOUT06\0308\

.

Data File Name

1780774B.D

Operator

23

Date Acquired

8/3/2006 19:14

Acq. Method File

MAN27

Sample Name

B 178/07 995474 TE

Vial Number

5

Calibration Title

Quantificati'On du rapport T/E

Last Calibration Update

Fri Aug 04 07:32:46 2006

#

Peak Tvoe Ret Time

Sianal Name

—

1)

•iSTD 20.99

301 .3 Methyltestoslerone

2)

18.57

432.4 Epitestosterone

L„..'

i r" -

3)

19.36
r^alriil Hi) rannnrf T/F

432.4 Testosterone

Target Response Amount Units

3356149 100.00 ng/mL

279871 5.75 ng/mL

3079122 61.64 ng/mL

i 1

Surface Concentration
11.0 10.7

Page 1 at 1

D:\MSDctiem\Custrpt\MAN27.CRT

S/4/20067;35AM ^^

USADA 0279

i '.

File: D:\Msd2 0\aout06\0308\l780774B.D

Operator: 2 3

Date Acquired: 3 Aug 2006 19:14

Instrument: MSD 20

Method File: ^4AN27

Sample Name: B 178/07 995474 TE

Misc Info:

Vial Number ; 5

I 1— J

Analyse quantitative : Testosterone /Epi testosterone

SI :METHYLTESTOSTERONE

2000000

TIC:1780774B,D

1500000

1000O0O

500000

1 1

1

rime-> 5.

/

iJJi

ij

ltui-ljL..jilUAy

^

^

-Jji-,jJ»"

... 1
DO 10.0

Q 15.00

20.00

liwndance Ion 301 .30 POI .00 to 302.00): 17a0774B.D

1O000O 21199

BOOOO

60000

40000 M.13

20000

21.22

rime-*

20,50 21.00 21.50 22.00 22.50

r-f

Epitestosterone -Testosterone

Mxindance Ion 432.40 (432.10 to 433,1 0): 17307748.0

11

SOOOO

60000

40000

2000O

8,11

18,57

^^^^19.62 ^

19,81

I3,8(

2Qa

3i

nme->

■!'''' !

18,50 19.00 19.50 20.00 20.50

Epitesto-Testo-llbetaOH A et E

i^jundance Ion 432.40 (432,10 to433,10). 17a0774B.D

«XXXX} Ion 522.50 (522.20 to gftCTQ): 17807746,0

300000

200000

100000

^m IK

19,81

20-11

page 1

USADA0280

5X

D:\MSD2D\AOUT06\0303\17S0774C.D

Data File Path

D:\MSD20\AOUT06\0308\

Data File Name

1780774C.D

Operator

23

Date Acquired

8/3/2006 1 9:45

Acq. Method File

WIAN27

Sample Name

B 178/07 995474 TE

Vial Number

6

Calibration Title

Quantification du rapport VE

Last Calibration Update

Fri Aug 04 07:32:46 2006

#

Peak Tvoe Ret Time

Sianal Name

1)

"ISTD 20.99

301 .3 Metliyltestosterone

2)

18.56

432.4 Epitestosterone

3)

19.37

432.4 Testosterone

Taraet Response Amount Units
4098783 100.00 ng/mL

329392 5.55 ng/mL

3670090 60.18 ng/mL

r':

Calcul du rapport T/E

n

Surface Concentration
11.1 10.8

55

Page 1 of 1

D:\MSDchem\Custrpt\MAN27.CRT

8^4/2006 7:36 AM

US AD A 0281

I '

File: D:\Msd2 0\aoutO6\030 8\l780774C.D

Operator: 23

Date Acquired: 3 Aug 2005 19:45

Instrument: MSD 20

Method File: MAN27

Sample Name: B 178/07 995474 TE

Misc Info:

Vial Number : 6

Analyse quantitative :Testosterone/Epitestosterone

SI :METHYLTESTOSTERONE

U

\bundance

TIC;1780774C.D
1

2000000

1500000

1000000

500000

/

ikil-lL^

iLuLiLl

IiUa,

J

In,

JduW

U

nme-> 5.

30

.. 1 1 1 1 1 I 1 . 1 I
10,00 15.00

20.00

Mjui

Ion 301 .30 (301 .00 to 302.00): 1 780774C ,D
2(199

TJme-5 20.50 21 .00 21.50 22.00 22.50

Epitestosterone -Testosterone

Abundance
100000

80000

60000

40000

20000

Time->

Ion 432.40 (432.10 to433.10);1780774C.D
ia37

„ 20.11
19.62

18,50 19.00 19.50 20.00 20.50

Epitesto-Testo-llbetaOH A et E

liundanoe Ion432.40 (432.10 to433.10): 17B0774C.D

Ion 522.50 (52220 to SitaO); 17807740.0

400000

300000

200000

100000

rime->

19.81

-r-r-' '■ [T-T-i-r- I I I I I I < I I I-,

13,50 19.00 19.50 20.00 20,50

page 1

USADA 0282

5lt

D:tMSD20WOt]T0eU130S\1780774S.D

r:

u

Li

Data File Path

Data File Name

Operator

Date Acquired

Acq. Mettiod File

Sample Name

Vial Number

Calibration Title

Last Calibration Update Fri Aug 04 07:32:46 2006

D:\MSD20\AOUT06\0308\

1780774S.D

23

8/3/2006 20:16

MAN27

B 178/07 995474 sshTE

7

Quanlification du rapport T/E

# Peak Type Ret Time Signal Name Target Response Amount Units

1) *ISTD 20.97 301.3 Methyltestosterone 3924981 100.00 ng/mL

2) 18.62 432.4 Epilestosterone 11645 0.44 ng/mL

3) ' 19.38 432.4 Testosterone 41499 1.22 ng/mL

Catcul du rapport T/E

r]

Surface Concenlration
3.6 2.S

Page 1 of 1

D:\MSDchem\Custrpt\MAN27.CRT

55

6/4/200S 7:37 AM

USADA 0283

File: D:\Msd20\aout06\0308\1780774S.D

Operator: 23

Date Acquired: 3 Aug 2006 20:16

Instrument: HSD 20

Method File: MAK27

Sample Name: B 178/07 995474 ssh TE

Misc Info:

Vial Number : 7

Analyse quantitative :Testosterone/Epitestosterone

U:

ri

Abundance

800000

600000

400000

200000

TIC: 1780774S.D

T— '

rime-> 5.00 10.00 1 5-00 20.00

SI :METHYLTESTQSTEROHE

Abundance lon301-30 301.00to302.00); 1760774S.D

100000 2C198

80000

60000
40000
20000

20.40

'mH^

rime">

70 m ai .00 21 .so 22.00 22.50

n

I :

f :

: I

u

Epitest oBterone-Testosterone

Laujndanc^ Ion 432.40 (432.10 to 433.10): 17807745.D

4000

3000

2000

1000

ri^o_> ia.50 19.00 19-50 20.00 MJO

Epi testo-Testo-lIbetaOH A et E
Abundance Ion 432.40 (432.10 to 433.10): 1780774S.D

Ion 522.50 (522.20 1o 523.20): 17807"^

5000

4000

rim.^> 18.50 19.00 19-50 20.00 20.50

page 1

5G

USADA 0284

File: D:\Msd20\aout06\0308\REFlTE.D

Operator: 23

Date Acquired: 3 Aug 2006 21:49

Instrument: MSD 2

Method File: MAN2 7

Sample Name: BLU + T30 E5

Misc Info:

Vial Number : 9

Analyse quantitative :Testosterone/Epitestosterone

r ";

Li

\bundance
250000

200000

150000

100000

50000

nme-> 5.00

TIC: REF1TE.D

10.00

15.00

_L»^

20,00

S I : METHYLTESTOSTERONE

Uundance
120000

1O0OOO
80000
60000
40000
20000

Ion 301 .30 (301 .00 to 302.00): REF1TE.D
2191

„ ;0. 13128211

O '^ i I I I I ' '

21.51

-J^

rime->

?n sn 71.00 21 -50 22.00 22.50

n

Epi testosterone-Testosterone
^bundarwe ion 432.40 (432.10 to 433.10): REFITE.D

50000
40000
30000
20000
10000

rime->

1£30

18.50
3^1

1 19.53

■Vr

■'-'-r

20.9

"M ' ' 'I

18,50 19.00 19 50 20.00 20.50

Plpit esto-Testo-llbetaOH A et E

k^indanci Ion432.40 (432,10 to433,10): REFnfc,D

Ion 522.50 (52330(63 523,20): REF1TE,D

50000
40000
30000
20000
10000

18,50
18

20,9

19,53

i I I 1 I I '

nme->

IBRD 19.00 19.50 20.00 20,50

page 1

5^

USADA 0285

Lj

If:

Pile: D:\Msd20\aoutt>6\0308\REF2TE.D

Operator: 23

Date Acquired: 3 Aug 2006 22:20

Instrument: MSD 20

Method File: MAN27

Sample Name: BLU + T180 E30

Misc Info:

Vial Number

10

Analyse quantitative :Testosterone/Epitestosterone

r ■
j

n

L:

u.

i^bundance
300000
250000
200000
150000
100000
50000

rime-> 5.00

TIC; REF2TE.D

1 . ii_lljL ^

10.00

15.00

"T
20.00

Epi t estosterone-Testosterone

^bjndarici Ion 432.40 (432.10 to 433.10): REF2TE.D

250000

200000

150000

100000

50000

rime->

IE 31

16.50

18.3as.62 18,97

19.52

20-9
-r-n

1B-50 19-00 19.50 20.00 20.50

S I : METHYLTBSTOSTERONE

^b^FdanM Ion 301 -30 (301 -00 to 302.00); REF2TE.D

2(191

BOOOO

60D00

40000

20000

n--eo-29

Till!'''

21.51

I i - i 'i'r i --r- i -^

ri„^^ 70 50 2V00 21.50 22.00 22.50

Kpit esto-Testo-llbetaOH A et E
^bjndanci lon432.40 (432,10 to 433.10); REF2TE-D

ffiOOOO Ion 522.50 {5233310 523,20); REF2TE,D

200000

150000

100000

50000

18-50
18-338,62 18,97

T

19-52

tc:n^> 18.50 19!00 19-50 2Q:oO 20,50

page 1

5^

USADA 0286

r'-

r"'

Pile: D:\Msd20\aout06\0308\REF3TE.D

Operator: 23

Date Acquired: 3 Aug 2006 22:51

Instrument: MSD 20

Method File: MAN27

sample Name: BLU + T360 E60

Misc Info:

Vial Number : 11

Analyse quantitative :Testosterone/Epitestosterone

SI :MET HYLTES TOSTEROHE
Kbundance

Ion 301,30 (301 -00 to 302.00): REF3TE.D
2d91

100000

80000
60000
40000
20000

„?0.1^B142

21.51

-/ | 'rrT'

nnie->

Tfl Rfi 21 .00 21 .50 22-00 22.50

I r;

1— :•

Epitestosterone-Testosterone

i^undance Ion 432.40 (432.10 to 433.10); REF3TE-D

1432

600000

500000

400000

300000

200000

100000

rime->

18-50

16.38,8.62 18.97

19,53

Ir'so' 'i9!oO 19.50 20.00 20.50

20.9

Epitesto-Testo-llbetaOH A et E

yjundance

600000
500000
400000
300000
200000
100000

Ion 432.40 (432,10 to 433.10): REF3TE,D
Ion 522.50 (52astl£) 523.20): REF3TE,D

18,50

18.3^8.62 18,97

19,53

20,33 20j

^

1B Rfl 19.00 19,50 2000 20,50

U

page 1

S^

USADA 0287

LNDD

ENREGISTREMENT

Code:
Version :
Date:

E-FCR-04B2
A

Q3/0S/2006

1/1

FICHE D' ANALYSE / RESULT AT - CONFIRMATION SEMI-QUANTITATIVE T/E (trob aUquotes)

Paraphe :
EchantilloD :

478/07 994474

432

Ion dc quantification Teste et Epitesto :

Concentration de la ttfSrence 1 : Testosterone:

Conccntratton de ta reference 2 : Testosterone:

Concentration de la r^ESrence 3 : Testosterone:

Dilution :
Ion de quantification SI :

30 Epitestosterone :

ISO Epitestosterone:

360 Epitestosterone :

1/ 1

301

5
30
60

T/E th6orique : 6
T/E thtorique : 6
T/E theorique : 6

Fichier

Surfece du SI

Surface Testosterone

Surface Epitestosterone

REFI

REFITE

3782021

1845917

294592

REF2

REF2TE

3011193

7S60237

1324358

REF3

REF3TE

3783290

20557109

3442296

1780774A

3971127

3733052

342595

1780774B

3356149

3079122

279871

I780774C

4098783

3670090

329392

RESULTAT DE L'ECHANTILLON

Fichier

1780774A

1780774B

I780774C

Movenne

Ecarttype

Valeur finale

Concentration Testosterone

63^

ng/mL

61,6

ng/mL

60,2

ng/mL

61,7

ng/mL

1,5

ng/mL

61,7

ng/mL

Concentration Epitestosterone

5,9

ng/mL

5,8

ng/tnL

5,6

ng/mL

5,7

ng/mL

0,2

n g/mL

Rapport T/E en surface

10,9

11,0

11,1

11,0

5,7

ngAnL

Seuil de declaration du report T/E ( en surface) :4 ^ o m/

Incertitude (iiee a la m«bode) pour le rapport T/E: 30^ pour Epitestosterone : 30/p pour Iji Testosterone : ^ A

Valeur basse du rapport T/E : T' T
Valeur haute du rapport T/E : l U ■ ^

Fartie a rempiir par le responsable

Bisuttat:

Anormal:

Inclassable :
Negatif:

4

Correction des concentrations en Testosterone et Enitestosterone par la density (cTAoc E-INC-03)

Numero du rSfractomtoe

Density afSchie

Pen site corrigte :

Facteur de correction

Concentration corrigee dc Testosterone

Concentration corrigfe d' Epitestosterone

:02s.

PARAPHE

— 2__

JQ

Ecartn":

Cet enregistrement est a archiver dans le dossier de confirmation

SO

USADA 0288

L.

LNDD

ENREGISTREMENT

Codification: E-CC-11
Version : B
Date: 08/03/2006
1/1

VERmCATION DES PEEPORMAKCfeS INSTRUMIISTALES EN CG/SM

Cscreening et confirmation)

Numero d'identification de I'appareU : M S b 2-^ .

Date: O'^/^^jo^-

1 -Source rt'innisation

MSD

Polaris

Autotime : Ion 69 ou 219 majoritaire
Autotime : Abondance de I'ion 502 > 3%
R^eller < 35
Ion time > 2 ms

Gui Xon

<"

<^

^

Observations :.

Lj

7 - EtancheVt^. du sVsteiiie

MSD / 18/69 ( H20), 28/69 (N2), 32/69 (02),-

Polaris
Observations :

Oui Non

44/69 (C02)< 10%
, Air et eau : Intemite ion 19 < intensity ion 18

S.

1 !

U

% - Sensibilite

Screening Recal / Mix conforme _ _
Conf TP conforme -Fichier: W ^

TP conforme - Ficbier '.

, TP con forms - Fichier j_-

— ■ TP conforme - r-ichi^i

TP conforme - Ficbier:

Observations :

Qui' Non

S

Code operateur etparaphe

.,(^^M-'(£

Cet enregistrement est

a archiverdans k classeur C-MA^Ech de I'appareU

USADA 0289

G'

r- :'

5973 Autotune

Instrument: MSD 20

Thu Aug 03 16:00:37 2006

D : \MSDCHEM\ 1 \5 97 3N\ ATUNE . U

Mass 69.0
Ab 483164
Pw50 0.62

Xi;

Mass 218.90
Ab 247349
Pw50 0.62

Mass 502.00
Ab 17083
Pw50 0.64

i:;;^

iv.

Ion Pol

POS

MassGain

397

MassOffs

-10

ArauGain

2576

AmuOf f s

127

Wid219 -

-0.O18

DC Pol

NEG

HED

ON

EMVolts

1353

Emission 34.6
EleEnergy 69.9
Filament 1

Repeller 30.46
lonFocus 90.2
EntLens 11.5
EntOffs 19.33

Samples 8

PFTBA OPEN Averages 3

StepSize . 10

Zones :

MS Source 230 Foreline

MS Quad 150

59

66

71 216

221 500

505

Scan: 10.00 - 700.00 Samples: 8 Thresh: 100 Step: 0.10
166 peaks Base: 69.00 Abundance: 439872

100 -1

80 -

60-

40 -

20-

j_k_

.^vW-

100

200

300

400

500

600

Mass Abund Rel Abund Iso Mass Iso Abund Iso Ratio

69.00 439S72 10 0.00 70.00 5101 1.16

219.00 230080 52.31 220.00 10123 4.40

502.00 15730 3.58 502.90 1442 9.17

USADA 0290

^

5973 Air and Water Check

:"i

L...

V

Li

Instrument: MSD 20

Thu Aug 03 16:05:12 2006

D : \MfiDCHEM\l\5973H\ATUNE.U

Scan: 10.00 - 75.00 Samples: 8 Thresh: Step: 0.10
64 peaks Base: 69.00 Abundance: 570752

100 n

90-

iO-

70 -

60-

50-

40-

30-

20-

10-

10

20

30

40

50

— r-
60

70

Mass

69.00 570752

18.10 11166

28.10 33960

Abund Rel Abund Iso Mass Iso Abund Iso Ratio

70.00 6224 1.09

19,00 68 .61

29.10 901 2 .65

100.00
1.96
5.95

Current Params used: ^^^„c

Rep =30.5 Entl = 19.33 Entr = 12 FOCUS

= 90 EMV = 1353

Relative abundances:
18/69 = 1.96
28/69 = 5.95
32/69 = 1.86
44/69 = 0.40
28/18 = 304.14

Water%
Nitrogen%
Oxygen%

Carbon Dioxide%
Nitrogen/Water%

US ADA 0291

"3

! 11

; i

p ■

File : D:\MSD2 0\AOUTO6\0308\TPTE.D

Operator: 23

Date Acquired: 3 Aug 2006 17:10

Instrument: MSD 2

Method File: MAN27

Sample Name: TP TE 2

Misc Info:

Vial Number : 2

Analyse quantitative :Testosterone/Epitestosterone

Abundance

■—.,

250000

,—.

200000

^

150000

1 ;
j \

100000

lJ

1"-

I 1

50000

rime-> 5.00

10,00

15.00

20.00

Epitestosterone -Testosterone

SI :METHYLTESTOSTERONE

^bundance
120000

Ion 301.30 (301 .00 to 302.00): TPTE.D
2C|93

100000

80000

60000

21.52

40000

20000

nme->

^,WBBBXXBSi

_ -^ - _

' f 1 — 1 1 [ 1 1 f '1 ' 1 1 — 1 — r p 1 — 1 T 1 ^-| 1 L 1 1 1 J 1 1 1

20.50 21.00 21.50 22.00 22,50

Epitesto-Testo-llbetaOH A et E

Abundance

Ion 432.40 (432
Ion 522.50 (52S

lOto 433.10): TPTE.D
30 to 523.20): TPTE.D

4000

;

20.;

3000

i8.a

8.63

2000

■1 63

1

1000

■'■'-jAA

j:A-..>—

19:§^fflS9 20-3420.62

jjL.^.^ —

rime~>

18.50 19.00 19.50 20.00 20.50

1

page 1

USADA 0292

6it