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2.4.2 Isotopic ratio analysis

USADA0152

Codification : M-AN
Version : B
Date :28/10/2005
1/2

-41

MODE OPERATOIRE D'ANALYSE POUR LA CONFIRMATION DE L'ORIGINE DES
METABOLITES DE LA TESTOSTF.BmVE PAR CPfi/r^MP, ^

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COLONNE

Type:
Longueur:
Diamitre interne:
ipaisseur du film:

INJECTION

Mode:

Temperature injecteur:
Volume inject^:
Solvants dc rinfage ALS:

CONDITIONS nc.

Temperature initiale:
Gradient de temperature;

Temperature finale;
Temps d'analysc:
Pression constante:

INTERFACE

Pi&ge i eau:
Ligne de transfeit;
Four k combustion:

coNPrnoNs sm

Mode d'acquisition:
Programmation de I'acquisittoQ;

DB17-MS JW Scien 122.4732

30m

0.25imn

0.25tun ASSURANCE QUALITY

LNDD

Splitless (insert splitless)

280*^

IfiMul

Solvant A: Acetonitrile

SolvantB: Hexane APPLICABLE

le

2 8 OCT. 2005

TO'C pendant 1 min
70->271»Ci30°C/min
271''G->281^ k 0.6»C/min
281°C pendant 3 mtu
281->300X4 5»C/min
300°C pendantSmin
45 min
Ajuster le SI i environ 870s

-lOO-C

SSCC

SSO'C

^%%

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ions 44, 45 ct 46

Tensps d'acquiqition total:2580s

a 100s RG open

il 30s RG close

k 160s RG open

& 190s RG close

a 220s RG open

i2S0sRG close

i 750s HS close

i 2000s HS open

i 2400s RG open

& 2430s RG close

& 2460s RG open

i 2490s RG close

& 2510s RG open

4 2540s RG close

USADA0I53

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Batch Data Processing Results

^r ta File Name

^^torun Setup File Name

Blank Subtraction
_Eac}<:ground Subtraction
""Reference Gas
..?ef Gas Delta iC13)

Ref Gas Delta (018)
^"urrent Time

Current Date

230706

230706

Disabled

Disabled

Enabled

-34.

-19.
21r23 :49
23/07/06

50
30

No.

Sample Details
Name

Elemental Isotopic

Weight Ref % Comp Delta
(mg) Type (C) (C13)

(018)

J

J

1 stabilite 1

2 stabilite 2
I 3 stabilite 3

4 Mix cal IRMS 003-1

5 Mix cal IRMS 003-2

6 Mix cal IRMS 003-3

7 Mix cal Acetate OOlA-lOOng inj

8 Blu 1 pool 4 F3/45U1 inj 2ul -

9 178/07 995474 F3/45ul inj 2ul

10 Blu 1 pool 4 Fl/SOul inj lul

11 178/07 995474 Fl/50ul inj lul

12 Blu r pool 4 F2/500U1 inj lul

13 178/07 995474 P2/400ul inj lul

14 Mix Cal Acetate OOlA-2

0.000 Sam

0.000 Sam

0.000 Sam

0.000 Sam

0.000 Sam

0.000 Sam

-31.51 -41.1

-32.22 -39.5

-31.59 -40.3

. 000 Sam

0.000.- Sam -30

O.OO'O Sam -3

0. 000 Sam -30

0.000 Sam -3

0.000 Sam -2

0.0 00 Sam

0.000 Sam

-25.21

--jNo.

J

J___

Sample Details
Name

Weight Ref
(mg) Type

Atom % Atom % XS
(C13) (C13)

! 1 stabilite 1

2 stabilite 2

3 stabilite 3

4 Mix cal IRMS

5 Mix cal IRMS

6 Mix cal IRMS

7 Mix cal Aceta

8 Blu 1 pool 4

9 178/07 995474
10 Blu 1 pool 4
il 178/07 995474

12 Blu 1 pool 4

13 178/07 595474

14 /lix Cal Aceta

003-1

003-2

003-3

te OOlA-lOOng inj

F3/45ul inj 2ul

F3/45ul inj 2ul
Fl/50ul inj lul

Fl/50ul inj lul
F2/500ul inj lul

F2/400ul ini lul
te OOlA-2

Sequence virifiie par : .li^.,

Remarques :

0.000 Sam
0.000 Sam
0.000 Sam
0.000 Sam
0.000 Sam
0.000 Sam

1.07659 -0.0346
1. 07582 -0 . 0354
1.07651 -0.0347

0.000 Sam
0.000 Sam

0.000 Sam
0.000 Sam
0.000 Sam
0.000 Sam
0.000 Sam
0;000 Sam

1.08310 -

1.07733 -0.

1.07699 -0

1.07809 -0.

1.07812 -0

1.07960 -0

1.07095 -

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Data Processing Results

DATA_010

230706

Blu 1 pool 4 Fl/50ul inj lul

5

0.0000
Sam
M-AN-41

micromass
13:11:34 Date
13 ;56 :19 Date

23/07/06
23/07/06

I ' Analysis of Reference Gas Data

L Ref Delta 13 = -34.50 Ref Delta 18 = -19.30

r, Time
1; 122. S
182.6
p., 242.7
'■ '■ 2423.5
L-' 2483.5
2533.5

u ■

Std Dev Of Fit

Major
8.633E-E
8.640E-E
S.674E-E
8 .603E-E
8.553E-e
8.S73E-e

Ratio 2/1
1.1780E-2
1. 1780E-2
1.1780E-2
1.1779E-2
1.1779E-2
1.1780E-2

1.5656E-7

Ratio 3/1
4.2529E-3
4.2531E-3
4.2530E-3
4.2523E-3
4 .2524E-3
4.2528E-3

1.9660E-7

U'

Analysis of Sample Peaks, with Background Subtraction

C02
! Time

L.;

Height

Area

2/1

3/1

dC13Pk dC13Bkd dOlBPk d018

867.0 3.68E-9 1.5642E-8 1.1815E-2 4 ,1787E-3

f 1473.5 3.27E-9 3.4193E-8 1.1885E-2 4.1658E-3

[_ 1763.2 1.29E-9 1.4952E-8 1.1865E-2 4.1785E-3

1826.6 3.77E-9 4.6201E-8 1.1879E-2 4.1729E-3

-30 .80 -58. 95

-24.55 -59.30

-26.44 -58.27

-25.16 -57.89

-36.42 15

-39.40 18

-36.43 17

-37.73 16

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i; Daia Filename: DATA_G10 Folder 230706

L: Date : 23/07/06 Time : 13:11:34

Comment : Blu 1 pool 4 FIBOui inj lul :
Parameters Automatic DP Params

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Data Processing Results

Data File Name
r-Folder

Sample Name
' Sample ID
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■ Injection Size
'Sample Type

Method
!"Batch Name
[ RunTime User

Acquisition Time
r Current Time

DATA Oil

230706

178/07 995474 Fl/50ul inj

lul

6

0.0000
Sam
M-AN-41

micromass

13:56:22 Date ; 23/07/06

12;23:08 Date ; 24/07/06

! Analysis of Reference Gas Data

L Ref Delta 13 = -34.50 Ref Delta 18 = -19.30

"! Time
1 122 . 6

Major

Ratio 2/1

Ratio 3/1

8

.557E-8

1.1780E-2

4.2530E-3

182.6

8

.541E-8

1.1779E-2

4.2529E-3

^- 242.7

8

559E-8

1.1779E-2

4.2528E-3

2423.5

8

570E-8

1.1780E-2

4.2528E-3

L- 2483.5

8

477E-8

1.1779E-2

4 .2526E-3

2533.5

' f

8

552E-8

1.1779E-2

4.2525E-3

Stci Dev Of

Fit

4 .6711E-7

1.1648E-7

Analysis of Sample Peaks, with Background Subtraction

.C02
I Time

(1

Height

Area

2/1

3/1

dCl3Pk dCl3Bkd dOlBPk dois

778

1

02E-8

5

1128E-8

1.178eE-2

4

1817E-3

-33

40

-55

27

-35

72

^

867

4

02E-9

2

3358E-8

1.1807E-2

4

1997E-3

-31

64

-54

92

-31

57

f.

881

6

2

OlE-9

1

9104E-8

1.1783E-2

4

2233E-3

-33

95

-54

82

-26

11

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1236

3

1

47E-9

1

4752E-8

1.1S68E-2

4

2016E-3

-26

35

-53

09

-31

14

9

1478

2

4

55E-9

5

1339E-8

1.1890E-2

4

1691E-3

-24

10

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64

-38

62

in

1764

6

1

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1

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1.1872E-2

4

1715E-3

-25

78

-49

65

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10

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2

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2

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1.1878E-2

4

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-25

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23

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Data Filename : DATA_On Folder 230706

Date :23/D7;0E Time : 13:56:22

Comment : 1 78(07 995474 F1 iSOul inj 1 ul :

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Data Processing Results

Data File Name
c -Folder
■ Sample Name
^"Sample ID
, Sample Position
; Injection Size
'-Sample Type

Method
' Batch Name
L RunTime User

Acquisition Time
-Current Time

DATA_012

230706

Blu 1 pool 4 F2/500ul inj lul

7

0.0000
Sam
M-AN-41

micromass

14:41:06 Date : 23/07/06

16:02:44 Date : 23/07/06

j i Analysis of Reference Gas Data

!_■ Ref Delta 13 = -34.50 Ref Delta 18 = -19.30

y

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Time

Major

Ratio 2/1

Ratio 3/1

122.5

8

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1.1779E-2

4.2525E-3

182.6

8

S46E--8

1.1779E-2

4.2529E-3

242. e

8

648E-8

1.1779E-2

4.2529E-3

2423 .4

8

572E-8

1.1779E-2

4.2526E-3

2483.4

8

565E-8

1.1778E-2

4.2526E-3

2533.5

8

561E-8

1.1779E-2

4.2529E-3

td Dev

Of

Fit

2.0409E-7

1.7605E-7

Analysis of Sample Peaks, with Background Subtraction

C02

Time

Height

Area

2/1

3/1

dC13Pk

dC13Bkd

d018Pk

d018

865.0

"■; 1231.7

; 1257.2

2.74E-9
4 . 52E-9
5.33E-9

1.4334E-8
3 .4e91E-8
4 .1709E-8

1
1
1

1S23E-2
1876E-2
ie80E-2

4
4
4

1667E-3

1668E-3

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-29.94
-25.34
-24.98

-65.47
-63.44
-63.15

-39.17
-39.15
-39.11

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Data Filename: DAT A_ 01 2 Folder ; 23070G

Date ;23ffl7/06 Time : 14:41:06

Comment : Blu 1 pool 4 F2600ul in|' 1 ul :

Paiameters Automatic DP Params

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r'lBatch Name
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^...Current Time

Data Processing Results

DATA_013

230706

178/07 995474 F2/400ul inj lul

0.0000

Sam

M-AN-41

micromass
15:25:49 Date
16:10:31 Date

23/07/06
23/07/06

I

Analysis of Reference Gas Data

LI

i Ref Delta

13

-34

50 Ref Delta 18

-19.30

Time

: 122.6

' 182.6

242.6

2423.5

2483.5

2533.5

8
8
B
S
8
8

Major
.603E-8
588E-8
578E-8
471E-8
452E-8
511E-8

Ratio 2/1
1.1780E-2
1.1779E-2
1.1779E-2
1.1779E-2
1.1778E-2
1.1777E-2

Ratio 3/1
4.2535E-3
4.2537E-3
4.2536E-3
4.2525E-3
4.2521E-3
4.2522E-3

Std Dev

Of

Fit

4.5694E-7

1.4227E-7

Analysis of Sample Peaks, with Background Subtraction

C02

C\ Time Height Area

2/1

3/1

dC13Pk dC13Bkd dOlSPk d018

Ll-

n

866.0 2.17E-9 9.6593E-9 1.1822E-2

1229.7 3.95E-9 3.1256E-8 1.1863E-2

1254.3 3.39E-9 2.5932E-8 1.1849E-2

1288.3 3.55E-9 2.9815E-8 1.1797E-2

4

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-30.07

-63.69

-38

44

18

4

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-26.43

-60.89

-39

38

18

4

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-27.71

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-38

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4

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-32.28

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Date :23/07J06 Time : 15:25:49

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Data Processing Results

DATA_0 08

230706

Blu 1 pool 4 F3/45U1 inj 2ul

3

0.0000
Sam
M-AM-41

micromass
11:40:11 Date
12 ;28 :05 Date

23/07/06
23/07/06

f"; ^ Analysis of Reference Gas Data

L; Ref Delta 13 = -34.50 Ref Delta 18 = -19.30

-. Time

Major

Ratio 2/1

Ratio 3/1

122.6

8

.660E-8

1 .1780E-2

4.2525E-3

182.6

8

.668E-8

1.17eiE-2

4.2527E-3

^ 242.6

8

e73E-8

1.1781E-2

4 .2531E-3

2423 .5

8

550E-8

1.1783E-2

4.2534E-3

i-' 248 3.5

8

558E-8

1.1782E-2

4 .2529E-3

2533.5

8

621E-8

1.1782E-2

4.2533E-3

y

d'

U-

Std Dev Of Fit 5.9183E-7 2.6505E-7

Analysis of Sample Peaks, with Background Subtraction
C02

.!-!■!- _.''!^^^' ''^^^ '/' 3/1 dC13Pk dC13Bkd dOlSPk d018

798.5 2.00E-8 1.2123E-7 1.1616E-2

867.4 6.17E-9 3.4892E-8 1.1822E-2

1244.7 2.49E-9 2.1148E-8 1.1848E-2

1306.2 7.10E-9 6.5412E-8 1.1854E-2

1336.6 2.32E-9 1.8245E-8 1.1845E-2

1375. G 1.42E-9 1.2239E-8 1.1852E-2

1651.5 3.59E-9 3.9165E-8 1.18e4E-2

4

.4640E-3

-50

.60

-61

70

29

47

q

4

.2211E-3

-30

.66

-62

20

-26

65

1 1

4

.1951E-3

-28

25

-63

83

-32

67

18

4

ie96E-3

-27

54

-63

93

-38

55

1 9

4

1806E-3

-28

40

-63

99

-36

03

1 P

4

1854E-3

-27

78

-64

02

-34

91

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1692E-3

-26

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File Edit View Calculate Report Parameters Status Help

Dala Filename ; DATA_008 Folder 230706

Date :23/07raE Time : 11:40:11

CommenI : Blu 1 pool 4 F3M5ljI inj 2ul :

Patameteri; Automatic DP Params

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Data Processing Main Graph

Graph Cursor Lines Window

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Current Time

D

Data Processing Results

DATA_009

230706

178/07 995474 F3/45ul inj 2ul

^ ■ I

0.0000 I

Sam

M-AN-41

micromass

12:24:59 Date : 23/07/OG

16 : 08 : 12 Date : 23/07/06

Analysis of Reference Gas Data
Ref Delta 13 = -34.50 Ref Delta 18 = -19,30

D

Time

122.6

182.6

,- 24 2.6

i 2423.5

U 2483. 5

2533 .5

Q

Major
8.494E-E
8.494E-E
B.494E-f
8.443E-f
8.453E-E
8.566E-E

Std Dev Of Fit

Ratio 2/1

Ratio 3/1

1.1782E-2

4.2529E'3

1.1782E-2

4 .2530E-3

1.1781E-2

4.2527E-3

1.17eOE-2

4 .2518E-3

1.1779E-2

4.2517E-3

1.1779E-2

4.2520E-3

1

5.6232E-7

r
1.7469E-7

*-;

Analysis of Sample Peaks, with Background Subtraction

u

n

C02

Time

Height

795.1

5.07E-9

827.1

2.21E-9

867.4

6.75E-9

1304.7

5.53E-9

1337.2

2.59E-9

1652 .

3-25E-9

Area

2/1

3/1

dC13Pk dC13Bkd dOlSPk dOlB

2.5669E-8 1.1S80E-2 4.2100E-3

1.0385E-8 1.1883E-2 4.2270E-3

3.0380E-8 1.1826E-2 4.1857E-3

4.6362E-8 1.1838E-2 4.1673E-3

2.1591E-8 1.1600E-2 4.1700E-3

3.7635E-8 1.1862E-2 4.1682E-3

■25.45
■25.34
-30.05
-28.82
-32.12

-55.46
-55.50
-55.38
-53 .62
-53 .42

-26.61 -51.12

-29.16
-25.22
-34.74
-38.95
-38 .31
-38 .72

5
6
7

11
12
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File Edit View Calculate Report Parameters Status Help

[j Data Filename : DATA_009 Folder : 2307D6

'-' Date : 23^7)06 Time : 12:24:59

Comment : 1 78/07 995474 F3H5ul inj 2u( : !

Parameters Automatic DP Params

Data Processing Main Graph

Graph Cursor Lines Window

1 .0OE-8t

S,00E-9-

6.00E-9-

1^
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e.ooE-s-

D.00E*O^

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-30,05

15.4B

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■25.34

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-32.12

.-26,61

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1. Tane

Specification : plateau du peack Centre > 10 V
Tune c.onforme :

out

non

2. Stability de rinstnim«nt

Sp&ification: 6cm mesuri entre valeur- n^ximale et valeuf fflinimale du ratio 2/1 < I
Stability oonforme :

duratio2/l<0.5%o

oxa\ V

non

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3. Prfe&ision de l'inst«^imi.iit . ,

Codede la solution BtoCairRMS:....,... Oq5

Valeaw nMc nues J%«VT iri nr 3Jniettinwy r

enne

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Code de la solution Mix Cal Acetate: ,..CaX

Valeiirs ohfenues (%n) -

DoiVa Q<i4^

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5a Androstanol AC

-So,iS

- 30|S€

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Valeiirs thdoriques + 0.5%q

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-30,46

-29.96

-30,96

Etiocholanolonc AC

.,19:91-

-19.41

-20.41

5b Andiostancdiol diAC

-33.81

-33:31

-34.31

Resultats conformcs :

11 KdtoetiocTiolanolone AC

-B.30

-1^80

■16.80

oui

bt

non

Observations;

RMultats : C0NF0RME/KOJ.^€ONFORME
Rayer la mention inutile

Validation

Op6rateur

Date

Code ct Visa

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Data. Pile Name
Folder
Sample Name
Sample ID
Sample Position
Injection Size
Sample Type
Method
Batch Name
RunTime User
Acquisition Time
Current Time

D^ta -Proceisimf -'^^uil^J

" -r _ ' •• . .''. ' '■■•

-DATA 0'03

230-706

stabilite

3

3
0.0000

Sam

C02-STAB

230706 -

micromass

09r50:48

Date

23/07/06

10:01:52.

P§t.e;.

23./0.77i!£

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Analysis of Reference Gas Data
Ref Delta 13 = -34.50 Ref Delta 18 =

-19.30

Time

42.5
102 .5
162.5
222.6
282.6
342.6
402.6
462.7
522.7
582.7

Std Dev Of Pit

n

r C02

Time Height Area

pi

t_'

Major

Ratio. 2/1

B

.459E-8 ■

1.17,e.iSE-2

8

.466E-8

l.l?:8®E-2

B

.456E-8

1.1780E-2

8

442E-8

1.1780E-2

B

499E-8

1.1779E-2

8

562E-8

1.1779E-2

8

627E-8

1.1779E-2

8

632E-8

1.1780E-2

8

640E-8

1.1780E--2

8

t

618E-8

1.17.80E-2

5 .2114E-7

Ratio 3/1
4.,2i49:8E--.3
4 . 2"4-9eE--?3
4 .2,4'54E-3
4..i4S4E-3
4.24-,9:&E-3
4..24-9-&E--3
4.2506E-3
4.2;§03|;-3
4.250iB-3
4.2511E-3

3.2526E-7

Analysis of Sample Peaks, with Zero Subtraction

2/1 3/1 dC13Pk d018Pk

i ■

u

US ADA 0177

^^C

■ a^ta- Prpceisi^ .^esyiji&i: .■ ■-■. '~ZM> ■^-'"

Data File Name

: a^TA..004-

.'.:.. ir^

Polder

■ -saovos

Sample Name

Mix cal IRMS 003

-1 ■: ■

Sample ID

Sample Position

1

Injection Size

0.0000

■

Sample Type

Sam

Method

M-AN-3 8

Batch Name

230706

.■ -

' ■■

RunTirrre User

micromass

. -

.. /': ' 'V ':■'

Acquisition Time

10:01:53

Darte :

23/0-7/06

Current Time

10: 17; 37

Rite :,

.23/£l,/j^

;,i-W'».--;-,3KJv*i.

Analysis of Reference Gas Data
Ref Delta 13 = -34.50 Ref Delta 18 = , -19.30

Time

42.6
102.5
742 .8
802.8

Major
, 584E-8
, 610E-8
.466E-8

551E-8

Ratio 2/1
1.1782Er2
1.178iLE-2
1.178-lE:-2
1.1780E-2

Ratio .3/1

4v25-l#-3
4.2SB-5E-3
4.2508E-3

Std Dev Of Pit

1.4024E-7

2.0412E-7

Analysis of Sample Peaks, with Zero Subti-actiori

2/1 3/1 dC13Pk dblSPk

C02

Time Height Area

n 190.1 5.97E-9 1.5080E-8 1.1797E-2 4.17^gE-3

Lj 255.7 4.55E-9 1.5439S-8 1.1844E-2 4.1835E-3

347.0 4 . 99E- 9 1 . 5465E- 8 1 . 1B03E-2 4 . 1717E-3

f- 533.3 4.5eE-9 1.4792E-8 1.1806E-2 4.156-5E-3

-32.52
-28.4.5
-31.96
-31.51

■-37.G.8
-35.0-4
-37.6-8
-41.13

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Data File Name

■ DfeTA 005 ■ ■■ . '^

Folder

2;3Q7p6

Sample Name

Mix cal IRMS 003-2

Sample ID

Sample Position

1 .

Injection Size

. 0000

Sample Type

Sam

Method

M-AN-38

Batch Name

230706

RunTime User

raicromass

Acquisition Time

10:17:39 Date : 23/07/0-6

Current, Time

10:4.8:38 Date : .2.3,/.P,7/p§

■„!tr.-:.

".. i j.fl>.-. ,.-,

i ( Analysis of Reference Gas Data

g Ref Delta 13 = -34.50 Ref Delta 18 = -19.30

r.
I ;
L,-

r

U

Time

42.6
102.6
742.8
802 .9

Major

8.531E-8

- 8.503E-8

8.519E-e

8.535E-8

Ratio 2/1
1.1780B-2
1.178iE^2
1.1781E-2
1.1781E-2

Ratio 3/1
4...251-.7E-3
4.2S1&E-3
4.251SE-3
4.2517E-3

.-..

i

Std Dev

Of Fit

1.1951E-7

1.2352E-7

W

Analysis of Sample Peaks, with Zero

Subtraction

C02

U

Time

Height Area

2/1 ■

3/1 dC13Pk

d018Pk

n

1

1

190.1
256.0
346.7
532.7

4.41E-9 1.0634E-
3 .29E-9 9 .B960E-
3.56E-9 1.0850E-
2 .94E-9 9 . 9025E-

-8 1.1793E-2
9 1.1845E-2

8 1.1801E-2

9 1.1804E-2

4
4
4
4

.1708E-3 -32.74

. 1762E-3 -28.28

.1747E-3 -32.13

1652E-3 -31.76

-37.95
-36.73
-37.07
-39.26

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Data Fiie Name
■- Folder
; Sample"\Hame
■■■■ Sample,, ID
^ Sample 'Position

Injection Size
■ . Sample 'Type

Method
r Batch "^ame
[^ RunTiTiie. User

Acquisition Time
T Curre.fit Time

■-- :'k'::^^.^

;l!iiBtta Processing

Re sill te

DMJA 006

230706

Mix cal IRMS 03

-3

1

0.0000

Sam

M-AN-38

230706

micromass

10:33:-24 Date :

23/07/06

10:49:07- Date :

23/07/06

-fiSim.

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Analysis of Reference Gas Data
Ref Delta 13 = -34.50 Ref Delta 18 =

-19.30

Time

42.5
102.5
742.8
802.9

Major
8 .547E-8
8. 56DE-8
8.464E-8
8.481E-B

Ratio 2/1
1 .178aE-2
1.178iE-2
1.17eiE-2
1.1780E-2

Ratio 3/1
4^2518E-3
-4.25.20E-3
4.2511E-3
4.2510E-3

Std Dev Of Fit

4.0299E-7 1.5020E-7

Analysis of Sample Peaks, with. Zero Subtraction

j 'C02
^ Time

Height

Area

2/1

3/1

dC13Pk dOiePk

190.1 5.78E-9 1.4231E-S 1.1796E-2

255.2 4.35E-9 1.4943E-8 1.1842E-2
346.5 4.74E-9 1.4336E-8 1.1803E'2
533.2 4.26E-9 1.3575E-8 1.1806E-2

4

.1698E-3

-32

56

-38

7?

4

-1838E-3

-28

65

-34

98

4

1712E-3

-31

95

-37

Sfi

4

1602E-3

-31

59

-40

36

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LJ

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Data File Name

Folder

Sample Name

Sample ID

Sample Position

Injection Size

Sample Type
Method
Batch Name
RunTime- User
Acquisition Time
Current Time .

"23U7Q6-

Mix cal Acetate OOiA-iOOng inj

2

0.0000
Sara
M-AN-41

micromass

10 : 53: 36 - Date

11:39:17 Date

u

k

23/07/06
23/07/06

Analysis of Reference Gas Data
Ref Delta 13 = -34.50 Ref Delta

18 =

-19.30

Time

122.5

182.6

242.6

2423.4

2483.5

2533.4

Major
8.6D9E-8
8.516E-8
8. 61,8E-8
8.509E-8
8.465E-8
8.S2BE-8

Ratio 2/1
1.17-8IE-2
1.17..81E-2
1.17-81E-2
1.1781B-2
1.1781E-2
1.1780E-2

Ratio 3/1
4.2S2aE:-3
.4.2522E-3
4.-2-5-23E.-3
4.251SE-3
4..25:i6E-3
4.2520E-3

',:- ^V'Y

- -^;

.--li^-^ n&^ji.

h- 1

L.i

r\

u

Std Dev' Of Fit

1.7125E-7

i.7134E-7

Analysis of Sample Peaks, with Background Subtracti

I ■

"-=

on

C02

Time Height

Area

^^^ 3/1 dC13Pk dC13Bkd dOlBPk d018

865.6 4.79E-3

1229. 8 4 . 79E-9

1302.2 3,63E-9

1473 . 8 3 .17E-9

2.0679E-8 1.1821E-2

3.7785E-8 1.1938E-2

2.8202E-e 1.1782-E-2

3.2254E-8 1.1976E-2

4

165.4E-3

-30

29

-6a. 4-7

-39

3 2

24

4

16S&E-3

-20

01

-6 6.70

-39

05

24

4

1663E-3

-33

70

-66.54

-39

OS

24

4

1665E-3

-16

69

-66.30

-39

06

24

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.':0ptli7ia GC 1.67-2 - E^^araisal DP

Data ■

Rlenarrie : DATA 007
Dale : 2mim

Comment :-Miji.,cSlfeetatet^l|ia:4^iTg;ir)i''! - ,-, ': ^ -r!^. ''^l3:J[:y:'- J ■'■;':!. -''..'■.' ' ^^■']-
Pararaetprs AutomatiG DP Pmm ■ - : ' £yii^.vf ^■■:,^r. v -Mi'f|f-I^ ^i;,:;^ J vi:-- .C -V ^.'^^.i:'- 1-- -'.Hj^^^-^.

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■"IMaJ^gcsssliig Maio Graplj

o jQ

::ineS

1 .odE^^

a,ooEs-

s.ooE-g-

E

4.00E-S-

2.00E3-

0.00E*o;

^-30.29 <;>-20.01

200

i-rrTT

400 600

X

"" 1 1 " i|

^-33.70 ■

<i>-16.69

'"''■ "^1 " 1 1 M I . I 1 1 1 1 1 1 M 1 w n ' n I rri-1-1

SOO 1000 i20D I-IOO 1600 1800 2000 2200 2400

I tulapri i

USADA0182

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Data Processing Results

Dai:c FiJs Name
Foider
Ssniple l\ame
Sanpic iZi
Sanpic iosicion
In'jecticn Size
Sample lype
Meuhod
Batch Natie
RunTime User
Acquisition Time
Current Time

DATA 014

23070S

Mix Cal Acetate

OClA-2

2

0.0000

Sam

M-AN-41

230705

micromass

20:39:04 Date

23/07/06

14 :24 ;44 Date

24/07/06

Ref

n

r-

i :

l:

Analysis of Reference Gas Data
Delta 13 = -34.50 Ref Delta 18 = -19.30

Time

Major

Ratio 2/1

Ratio 3/1

122.6

-8

663E-8

1 . 1777E-2

4.2533E-3

182.6

e

686E-e

1 . 1778E-2

4.2533E-3

242.6

8

696E-8

1.1777E-2

4 .2538E-3

2423 .5

8

634E-8

I.1776E-2

4.2523E-3

2483.5

8

613E-8

1.1776E-2

4 .2525E

-3

2533.4

8

550E-e

1.177eE-2

4.25302

-3

p Std Dev Of Fit 2.3526E-7 3.3G47E-7

""" Analysis of Sample Peaks, with Background Subtraction

r"-

C02

i-- Time Height Area

2/1

3/1

dC13Pk dC13Bkd dOlSPk d019

f"1

u

866.6 4.03E-9

1228 .5 4 . 07E-9
1301 , 3 .09E'9

1471 . 6 2 .60E-9

1.7744E-8 1.1814E-2

2 . 9964E-8 1. 1932E-2

2 .3587E-e 1 , 1776E-2

2.6828E-8 1.1972E-2

4

1663E-3

-30

55

-69

16

-39

38

24

4

1584E-3

-20

22

-65

52

-38

89

24

4

1712E-3

-33

90

-55

65

-3a

19

24

4

1715E-;3

-16

.76

-67

09

-3B

15

24

L^

US ADA 0183

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D

n

L

n
[j

D

n

u

G

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M

D
[J

L.

^.6I?^?.r Manuat^DP

File Edit View Calculate Report Parameters Status Help

Data Filename : DAT A_C1 4 Folder : 230706

Date : IMJIOS Time : 20:39:04 ;

Comment : lv1iKCalAcelateO01A-2: 230706 |

Pacameters Aulomatic OP Params

Graph Cursor Lines Window
1 oi:iE-St

SQOEa-

c'.C0£3-

a.

4.0CIE-Q-

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-30,56 .,.-20.22

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£'30 4CiO 500 ^00 HSOO 1^00 14CiO 1500 ISOQ SOCO 2200 2400

Sees

USADA0184

M3>

r-
t '

I.'

S

r

rt

M

LNDD

ENREGISTREMENT

Codification : E-FCR-06

Version : E

Date :24/l 1/05

Page : 1/2

FICHE D'ANALYSE / RESULTATS GC/C/IRMS

Echantilloii :
Repertoire:

178/07 995474

230706

Instrkiment : GC/C

CO et paraphe:

S Isoprime I

Valeur isotopique du reactif de derivation:

-53

Fraction Fl fmetabolites de la cortisone et du cortison

Blanc urjnaire

Echantillon

SI

1 1 K6lo6tio

SI

1 1 K6toaiD

Nom du fichier

Data 010

Data 010

Data Oil

Data Oil

tr(s)

867

1474

867

1478

trr

-

1.700

-

1.705

Intensity (nA)

3.7

3.3

4.0

4.6

5 ' C %o mesuree

"30.80

■24,55

, -31.64

-24.10

5 ''C %o corrigde

-

-21.56

1
1

-21.06

Fraction F2 (Ketos)

Blanc urinaire

Echantillon

SI

Etio

Andro

SI

Elio

Andro

Nom du fichier

Data 012

Data_012

Data 012

Data 013

Data 013

Data 013

tr{s)

868

1232

1257

866

1230

1254

trr

-

1.419

1.448

1 ' — — —

1.420

1.448

Intensity (nA)

2.7

4.5

5.3

2.2

4.0

3.4

6 "C %o mesuree

-29.94

-25.34

-24.98

-30.07

-26.43

-27.71

6 '^C %, corrigae

■

-22.43

-22.03

1

-23.63

-25.05

Fraction F3 (D

Ob)

Blanc

urinaire

SI

5p Adiol

5 a Adiol

' 5P Pdio!

Nom du fichier

Data_008

DataOOS

Data 008

Data 008

tr{s)

867

1305

1337

1652

trr

-

1.506

I.S41

1.904

Intensity (nA)

6.2

7.1

2.3

3.6

5 '^C %B mesuree

■30.66

-27.54

-28.40

-26.65

8 "C %o corrig^e

-

-22.18

-23.22

-21.63

Echantillon

Si

5P Adiol

5a Adioi

5P Pdiol

Nom du fichier

Data 009

Data 009

Data 009

Data 009

tr(s)

867

1305

1337

1652

trr

-

1.504

1.542

i.905

Intensity (nA)

6.8

5.5

2.6

3.3

5 '^C %o mesurSe

-30,05

-28.82

-32.12

-26.61

5 "C %o corrtgee

-

-23-73

-27.72

-21.58

USADA0185

^-94

r

i '

■A

-j\

LNDD

ENREGISTREMENT

Version : E

Codification : E-FCR-06

Date: 24/1 1/05

FICHE D' ANALYSE / RESULTATS GC/C/IRMS

Page : 2/2

1

1
1

valeur de reference d'une population t§moin'

Echantillon

dans les normes

6 "C %o haute

fi '^C %o basse

oui

non

1 ! Ketoetio

-17.58

-26.27

V

Etio

-19.56

-26.10

^ .^ ,

X

Andro

-18.43

-25.02

X

5P Adiol

-18.55

-26.97

X

5a Adiol

-18.59

-27.40

X

5P Pdiol

-18.25

-25.55

V

Blu

Echantillon |

A%<,

A%o + 0,89So

A%o

A%o - 0,8%o

Etio - 1 1 Ketoetio

-0.87

-1.78

-2.58

-3.38

Andro - 1 ! Ketoetio

-0.48

-3.19

-3.99

-1.79

Sp Adiol- 5(5 Pdiol

-0.55

-1,35

-2.15

-2.95

5a Adiol -5p Pdiol

-1.59

-5.34

-6.14

-6.94

Seuil de nositivite de TAMA : 5'^C%o(metabolite) - 5'^C%o{compose endogene de reference) > 3S6o

S'^C du compose < -28%o
Variation maximale admissible liee a la methode: +/- 0,8%o

Conclusion

L'analyse de I'echantillon par spectrometrie de masse de rapport isotopique (EC3 1) indique une
origine exogene des metabolites de la testosterone, coherente avep une prise de testosterone ou de
!'un de ses precurseurs. j

L'origine exogene des metabolites de la testosterone a ete objectivee sur la base d'un
appauvrissement isotopique de 3.99%o et 6.14%o, respectivement pour les metabolites androsterone
et 5a androstanediol.

Paraphe du responsable;
Observations:

C^

Partie a remplirpar le responsable

USADA0186
Ecart(s) n" :
Cet enregistremeni est a mettre dans le dossier de confirmation ,^,yf^ ^