LNDD MODE OPERATOIRE Codification : M-AN -41 Version : B Date :28/10/2005 1/2 MODE OPERATOIRE D'ANALYSE POUR LA CONFIRMATION DE L'ORIGINE DES METABOLITES DE LA TESTOSTERONE PAR CPG/C/SMRI r ■ i i I i ^ I \ I u Q f L L; r COLONNE Type: DB17-MS JW Scien 122.4732 Longueur: 30m Diamitre interne: 0.2Smm ,«.,..,%...«.-_ Epaisseur du film: (j^5 ASSURANCE QUALITE LNDD INJECTION Mode: Splitless (insert splitless) Temp^tiiTc injecteur: 280"'C Volume inject^: luMul Solvants dc rinfage ALS: Solvant A: Ac^tonitrile So!vantB:Hcxane APPLrCABLE 1 CONDli'IONS GC . 280CT. 2005 Temperature initialc: 70°C pendant 1 mtn Gradient de tenq>6rature: 70->271°C4 30°C/min 271°C->28rC k 0.6=C/min 2SrC pendant 3 min 281->300''Ca5<'C/min Temperature finale: Temps d'analyse: SOCC pendant5niin^i^^iL, 45 niin "^-^-^ Pression constante: Ajuster le SI & environ 870s INTERFACE Piegc k eau: -100-G ^rs\M\P^ Ligne de transfert: 'Z% sPt"^^^^ Four k combustion: CONDITIONS SM Mode d'acquisition: ions 44, 45 et 46 Programmation de I'acquisition: TcnqK d'acquiqition total:2580s ^ 100s RG open & 130s KG close & 160s RG open i 190s RG close & 220s RG open &2S0sRG close i 750s HS close i 2000s HS open & 2400s RG open & 2430s RG close i 2460s RG open & 2490s RG close &2S10sRGopen k 2S40s RG close USADA 0329 Uoo LNDD MODE OPERATOIRE Codification : M-AN -41 Version : B Date :28/10/2005 2/2 MODE OPERATOIRE D'ANALYSE POUR LA CONFIRMATION DE L'ORIGINE DES METABOLITES DE LA TESTOSTERONE PAR CPG/C/SMRI iMiiHittifeffiiiftfli llflil>ii1Nllit^l1lill!l''ii|l|'lltl'IIWIIilMIII||l|')y'llllMlllM redig^par Cynthia MONGONGU 28/10/2005 jh??!^ veriii^par Caroline BASTIEN 28/10/2005 ^ L 1 -^ verifi6par Aurfiie LAURENT 28/10/2005 ' rn 1 approuv^par Jacques DE CbAUREIZ, 28/10/2005 /fm^l^ U-' N° Version Motif Date 1 Creation du document. 27/05/2002 A Acceptation du projet ^res conversion du tr du SI en seconde, creation de la version A 14/10/2002 B Revision biennale 28/10/2005 SPECIMEN L; USADA 0330 Jo-i Batch Data Processing Results Data File Name Autorun Setup File Name Blank Subtraction Background Subtraction Reference Gas Ref Gas Delta {C13) Ref Gas Delta (018) Current Time Current Date 04080S 040806 Disabled Disabled Enabled -34. -19. 22:17:03 04/08/06 50 30 Mo. Sample Details Name Elemental Isotopic Weight Ref % Comp Delta (mg) Type. (c) (ci3) (018) n i I t — ' 1 Stabilite 1 2 Stabilite 2 3 Stabilite 3 4 Stabilite 4 5 Stabilite 5 6 Mix Cal IRMS 7 Mix Cal IRMS 8 Mix Cal IRMS 9 Mix Cal Aceta 10 Blu 1 Pool 4 11 178/07 995474 12 Blu 1 Pool 4 13 178/07 S95474 14 Blu 1 Pool 4 15 178/07 995474 16 Mix Cal Aceta 003-1 003-2 003-3 te OOlA-1 F3/4 5UL i F3/4 5UL F1/120UL Fl/lSOuL F2/14 00UL F2/850UL .te OOlA-1 .000 Sam .000 Sam 000 Sam 000 Sam 000 Sam O.OOC Sam -31 ^n -40. .000 Sam -31 fiR -40. D -OOng inj 0. 000 Sam 0.000 -31 Sam 42 -39.3 nj 2uL inj 2uL C .00 Sam 0,00 Sam -31 -3 -3 inj 2uL 0.000 Sam inj 2uL 0. 000 Sam inj 2uL 0.000 Sam inj 2uL 0.000 Sam OOng inj 0.000 ■Sam Sample Details No . Name Weight Ref (mg) Type Atom % Atom % XS (C13) (C13) 1 Stabilite 1 2 Stabilite 2 3 Stabilite 3 4 Stabilite 4 5 Stabilite 5 6 Mix Cal IRMS 003-1 7 Mix Cal IRMS 003-2 8 Mix Cal IRMS 003-3 9 Mix Cal Acetate OOlA-lOOng inj 10 Blu 1 Pool 4 F3/45UL inj 2uL 11 178/07 995474 F3/45uL inj 2uL 12 Blu 1 Pool 4 F1/120UL inj 2uL 13 178/07 995474 Fl/l50uL inj 2uL 14 Blu 1 Pool 4 P2/1400UL inj 2uL 15 178/07 995474 F2/850uL inj 2uL IS Mix Cal Acetate OOlA-lOOng inj 0. 000 0.000 0. 000 0.000 0.000 0.000 0.000 0.000 Sam Sam Sam Sam Sam Sam Sam Sam 1.07683 -0.0344 1.07641 -0.0348 1.07670 -0.0345 0-000 Sam 0.000 Sam 0.000 Sam 0.000 Sam 0.000 Sam 0.000 Sam 0.000 Sam 0.000 Sam 1.08114 - 1.07712 -0. 1.07560 -0 1.07649 -0 1.07751 - 1.07826 - 1.07131 - 1.08271 - USADA0331 UOS; r- g f I r- u n u n D u Lj U u cy .J in 7, o irt- fl S « ■n c ro £ ■D u •Si r4 7. tr c u < JJ Q rri u c ra iH •l-l u UJ V) b. rH 3 a ^ H J3 rH □:> o IC Qi ^ (\ o H ^ w VO H (U o u 4J ■r\ 3 vo m n o c rf o ■H ■' ft H U r>j (N t 3 Csl CTUN Tl 3 Q H U m a. V) C E X 3 ffl ^ 10 "T ■H .-( ,. CM IQ III T a tl k4 4J £ c m a u -n ID Z 14-1 g 11) F C 3 U iJ 3 IP H 2 nj -H 1m H Q) H 3 JJ a u -H H (1) C W B 3 ^ L_- USADA 0332 .-103 r. File hdil View CalcxilBie R^o!^^SS^S!^Sp Dstfi Rename :DATA_012 Polde, : 040806 Date :04^08raG Time :18-33-24 Comment : B ki 1 Pool 4 Fl /1 20uL in; 2uL ■ Parameters Automatic DP Patams n u Graph Cursor Lines Window 1.00E^, 'iJ e.ooE-9 6.00E«- 2L I 4,00E-9- 2.00E-9- L. u O.O0E-«^ 200 400 -30.45 y~JK,^_)_ * -24.56 BOO eoo 1000 ■f£00 1400 Sees o roi " a ( : USADA 0333 Jc/f THERE WAS NO PAGE 105 IN THE ORIGINAL DOCUMENTATION PACKAGE. THIS PAGE IS INTENTIONALLY LEFT BLANK USADA 0334 Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position Injection Size Sample Type Method Batch Name ■RunTime User Acquisition Time Current Time DATA__012 040806 Blu 1 Pool 4 F1/120UL inj 2uL 5 0.0000 Sam M-AM-41 micromass 18:33:24 Date : 04/08/06 19:ia;07 Date : 04/08/06 Ref Delta 13 = Analysis of Reference Gas Data -34.50 Ref Delta 18 = -19.30 Time Major Ratio 2/1 Ratio 3/1 122.6 8 532E-8 1.1773E-2 4.2515E-3 182 .6 8 541E-8 1.1773E-2 4.2517E-3 242 .6 8 493E-8 1.1773E-2 4.2515E-3 2423 . 5 8 .481E-8 1.1773E-2 4.2516E-3 2483 . 5 8 .479E-8 1.1773E-2 4.251SE-3 2533.5 8 Fit .517E-8 1.1773E-2 1.3906E-7 4.2520E-'3 1.7907E-7 ■~N n Analysis of Sample Peaks, with Background Subtraction U C02 Time Height Area 2/1 3/1 dC13Pk dC13Bkd dOlSPk d018 9.0004E-9 1.1813E-2 4.1841E-3 -30.45 '64.35 -34.89 18 '''-' l:lltl 3:o458e:8 i:i8;;s-2 i■.l..^-l -^-n -^.i^ -3^." ^0 1489 .8 1843:5 3:29E:; 3:8;o;E-8 1.1864E-2 4.1725E-3 -25.95 -58.90 -37.61 18 Li I : ! t U Jc^ USADA 0335 I" ', i L' k^l N in 1 O 1 J '. 1 u z s 1 ■0 J h- n o g u 111 s o I- ■ L . c Li U-l I- c r-l t""t O 3 C L. CD [-■ H y -d U f' CO U' o H fei bi *3 i': ■ VO H ■w r- O r~ ■v 1 4J rr ifi U' 3 ID o < o r\ . (M (J'M f~ I"- L.. T3 3 3 O O K) fC Ul-^^ E S 03 CO f ' ^ ic ^ r- r- J .. OJ H H in '. 1 D 11 u 4J g H) 1 i c a Si ' 1 htD D Z IJ b Li 11 g c 3 4J U 3 11 M ■.i nj -H l4 rt HI !■ 3 4J Q, U ■-I rH 0) C men ID ■ ! .H ac C ffl-^ ■rl L_f 111 < H tn s > CD CJ O X IN IN -1 OJ ^ r' USADA 0336 Jt? ■^ ©ptima GC 1.67-2 - Manuai DP File Edit View Caicutate Report Parameters Status Help Data nieriame:DATA_013 Folder : 04D806 Dale : 04/08/06 Time : 19:18:09 Comment : 1 76/07 995474 Fl /1 50uL inj 2uL Parameters Automatic DP Params □ rDi Data Processing Main Graph Graph Cursor Lines Window l_i 6.CI0E5- r] U o n 6.00E-9- 8. < 4.00E-9- 2.00E-9- 0,OCiE-tfr, .-S3. 64 -24.75 _i . ITYTT^.^.fTrrVT , 11.1 . ■ .II M I..!,..- , I I mT i TTT i T I|.M.J | i S l M ^-l -l 2CiO 400 500 SOO 1000 1200 1400 1600 1SO0 2000 2200 2400 I Major Sees L-( u USADA 0337 M Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position Injection Size Sample Type Method Batch Name RunTime User Acquisition Time Current Time DATA_013 040806 . . _ T 178/07 995474 Fl/150uL in:) 2uL 6 .0000 Sam M-AN-41 micromass 19:18 l09 Date 08:07:48 Date 04/08/06 05/08/06 ■~\ Analysis of Reference Gas Data " Ref Delta 13 = -34.50 Ref Delta 18 = -19-30 L-,: Time 122.5 182.6 242.7 2423.5 2483.5 2533.5 Major .495E-B .501E-8 .541E-8 .495E-8 .456E-8 . 598E--8 L:std n Ratio 2/1 1.1774E-2 1.1773E-2 1.1773E-2 1.1775E-2 1.1775E-2 1.1775E-2 3.6976E-7 Ratio 3/1 4.2514E-3 4.2514E-3 4.2517E-3 4.2521E-3 4.2522E-3 4.2528E-3 2.8218E-7 Dev Of Fit ,is of sample Peaks, with Background Subtraction Analys] C02 T' Time Height Area 2/1 3/1 dC13Pk dC13Bkd dOlSPk d018 7 n I ill 9 2 84561-8 1.1879E-2 4.1846E-3 70.2 90.1 ■33.64 -129.52 -31.08 -122.87 -24.75 -127.77 -37.95 63 -29.33 42 -34.88 58 D I" 'i USADA 0338 JQ5 f=^ n u U n U n n a r 1 Li i U z rt z V c 4-1 a> E IT U < D Cn C M --I 4-1 in H 3 3 H y CO o o o l-l 3 1 ■ I US ADA 0339 JAo r'- u File Edit View Calculate Report Parameters Status Help L-J Data f Parameters Filenart\e:DATA_014 Date : 04?08;OG Fdder : 040806 Time : 20:02:53 Comment : Blul Pool4F2/1400ii-ii^2uL Automatic DP Pat ams |>3l3 f^ocessing Main Graph r^ Graph Cursor Lines Window i i !' I 8.00E-9- 6,O0E-g- n. £ < 4,0OE-9- 2.00 E -9- O.OOE+0 ^-24.63 -25.54 <> -30.47 I ■■ v ' ^' ■ ^ - 200 400 D IDl = a liulapr T" ...I l l '' I I . I . . I ■ I ■ I I . V 600 SOO 1000 1200 1400 Sees ■ I ■ " T- -1500 1S00 2000 2200 2400 }U USADA 0340 Data File Name Folder r- Sample Name i Sample ID Sample Position . Injection Size ] Sample Type '■ ^Method Batch Name r [RunTime User [ Acquisition Time Current Time I i Data Processing Results DATA_014 '. 040806 Blu 1 Pool 4 F2/14D0UL inj 2uL 7 0.0000 Sam M-AN-41 micromass 20:02:53 Date 08:18 :20 Date 04/08/06 05/08/OS Analysis of Reference Gas Data Ref Delta 13 = Time r 122.6 [. 182.6 242.6 . .2423.5 1 :2483.5 ^■2533.5 LJtd Dev Of Fit j-1 Analysis of Sample Peaks, with Background Subtract 1 r to2 ^, Time Height Area - J^ . 3u Ker ueita 1 8 = -19.30 Major Ratio 2/1 Ratio 3/1 496E-8 1.1776E-2 4.2531E-3 503E-a 1.1776E-2 4.2531E-3 494E-8 1.1776E-2 4.2528E-3 442E-8 1.1774E-2 4.2519E-3 385E-8 1.1774E-2 4.2515E-3 462E-8 1.1773E-2 4 .2518E-3 3.6403E-7 1.7354E-7 ion ?^^ ^/l dC13Pk dC13Bkd dOlSPk d018 L- 869.0 2.38E-9 1 . 2861E-8 1 . 1814E-2 4.i675E-3 1241.0 3.05E-9 2 . 4953E-8 1 . 1870E-2 4.1678E-3 -30.47 -25.54 -71.51 -68.90 -38.95 -38.86 r.267.5__3.48E-9__2.7395E-8 1.1880E-2 4:166;E-3 -Hisl :68:70 lH] 06 27 27 27 u USADA 0341 M^ I I I I I - r; (■; l"! -L r- j i r r w 1 Q Z l&j rt ? E ■s ■D ij J ^ j: a 4J o u o S ■5- Q tr u n CM 'C c "H ID ^ D> T3 t- c ■qi -H CM r~ w O 3 c CD f- -H H 4J y y CO ^ \0 ^ (- 1- ,. (NJ iH rl l~ D Ql u u E Ql c HI i! ^ Ti az'*^ E 11 B C 3 4J H 3 HI M 2 ID -ri IjH 0) H 3 u 0, U H H n ff m £ i" (D -H a.u C IT! -H ■^ lu rt H w E ? USADA 0342 M^ r ■ Ul- (MimsGC 1.6/-2 - Manual DP File Edit View Calculate Report Parameters Status Help u. r I r lJ i I ! i 1 I Date Filename :DATA_01 5 Folder : 040BDB Dale : 04108^6 Time : 20:47:38 Comment : 178/07 995474 F2l850uL inj 2uL Parameters Automatic DP Params Data Processing Mam Graph Graph Cursor Lines Window e.ooE-3- 6-O0E-9- E 4.00E-9- I . £,0OE-9- L.. C.OOE-h:^ _Jl^-L-' -30.00 y^^^j ■27.93 \J- J^ U_kJ. Q IDI ° D Iculapr 200 400 600 fiOO 1000 1200 1400 1600 1600 2000 2200 2400 Sees u USADA 0343 Mii Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position Injection Size Sample Type Method ! Batch Name ■RunTime User Acquisition Time Current Time DATA_015 040806 178/07 995474 F2/850uL inD 2uL 0.0000 Sam M-AN-41 micromass 20-.47:38 Date 08;03;23 Date 04/08/06 05/08/06 Analysis of Reference Gas Data Ref Delta 13 = -34 .50 Ref Delta 18 = -19.30 Time „ 12 2 6 182 5 ''• 242 5 i ■ 2423 4 2483 5 .- 2533 5 Major 8 . 556E-8 8 .604E-8 8 .602E-8 8.506E-8 8.522E-8 8 .602E-8 Ratio 2/1 1. 1774E-2 1.1775E-2 1.1775E-2 1.1773E-2 1.1773E-2 1.1773E-2 Li Ratio 3/1 4.2526E-3 4.2533E-3 4.2537E-3 4.2517E-3 4.2517E-3 4.2523E-3 4 . 96G2E-7 Std Dev Of Fit 5.2841E-7 ; Analysis of Sample Peaks, with Background Subtraction ■C02 Time Height Area 2/1 3/1 dC13Pk dC13Bkd dOlBPk d018 L- 870 1 3 47E-9 1.6473E-B 1.18iaE-2 1241 1 4.00E-9 3.2334E-8 1.1856E-2 ncc Q 7 q7E-9 2 1992E-8 1.1841E-2 1301:9 Isll-l 3:i072E-8 1.1791E-2 4.169eE-3 4 ,1661E-3 4.1657E-3 4.1682E-3 ■30.00 -26.58 -27.93 -32.37 -65.04 -61.51 -60.71 -59.44 -39.32 -39.38 -38.79 -38.45 21 21 21 20 I L u n USADA 0344 MS r , r; u- S g < '■■' t 2 }"• 1 O z < o 3 ■c C XJ "^ "J U £ ■D i- i 4J 0- n c w -H LJ U a c m ■H u r-l [i. L H a ^ H f- 1 1 ^ a 1 : o (M Oi 1 — o rH J o H ■H u- 3 10 0] o C «; o ■H ^ N tr ^J Csl IN U. 3 t IN tJilM TJ 3 Q rt U m < M c z z 3 ni y Ifl ^ H H ^ Q c\ CO can 11) ^ U F 01 c m D 1 M -0 01 2 "H E ■'-' lu e C 3 4J >J 3 01 H Z (P lO --1 IH H , 111 M 3 4J a u H q H m 0" n E m c] "o c ■H a u c m ■-f ■-) D Ck T w w s > < < c. -.-s USADA 0345 JJ'^ r i . u L r. f I D L L. L 1 1 file Edit View Calculate Report Parameters Status Help Data Filename: DAT A_mO Folder : 0408D6 Date ■,04ra8IQ6 Time : 17:03:53 Comment : Blu 1 Pool 4 F3(45vjL inj 2uL : Paramctets Automatic DP Paiams Bata Processing Main Graph Graph Cursor Lines Window S.OOE-Q- 6.00E-9- E < 4.00E-9- 2.00E-9- O.OClE-tCuVrTW 200 400 600 □ IDI ° a Irulagr eM 1000 1 200 i 400 1 600 iSOO 2000 2200 2400 Sees USADA0346 M7- Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position .Injection Size Sample Type Method iBatch Name ^RunTime User "Acquisition Time Current Time DATA_010 040806 Blu 1 Pool 4 F3/45UL inj 2uL 3 0.0000 Sam M-AN-41 micromass 17:03 :53 Date : 04/08/05 07:47:30 Date : 05/08/05 Analysis of Reference Gas Data ■ Ref Delta 13 = -34.50 Ref Delta 18 = -19.30 Time Major Ratio 2/1 Ratio 3/1 122 . 6 8 .545E-8 1.1774E-2 4.2514E-3 182 . 6 8 537E-8 1.1773E-2 4 .2513E-3 242 . 7 8 497E-8 1.1773E-2 4.2507E-3 2423 . 5 8 468E-8 1. 1772E-2 4.2505E-3 2483 .5 8 400E-8 1 . 1772E-2 4 .2507E-3 2533.5 8 435E-8 1.1772E-2 4.2508E-3 ^td Dev Of Fit 3.7547E-7 2.7523E-7 ; ; Analysis of Sample Peaks, with Background Subtraction C02 r; Time U 1 - Height Area 2/1 3/1 dC13Pk dC13Bkd dOlSPk d018 799 1 35E-8 5 .8132E-8 1 1877E-2 4 1762E-3 -24 77 -67 24 -36 59 17 r-' 872 4 5 30E-9 2 2912E-8 1 1801E-2 4 1836E-3 -31 54 -55 95 -34 88 17 ■ 881 1 2 34E-9 1 2956E-8 1 1867E-2 4 2171E-3 -25 01 -66 81 -27 15 17 '■-12 6 3 2 49E-9 2 2592E-8 1 1843E-2 4 1987E-3 -27 91 -55 40 -31 37 19 1323 r 7 D4E-9 6 5008E-8 1 1845E-2 4 1705E-3 -27 54 -65 35 -37 87 20 ■ L353 8 1 98E-9 1 6534E-8 1 1838E-2 4 1904E-3 -28 31 -65 37 -33 27 20 I_i394 3 1 68E-9 1 5157E-8 1 1844E-2 4 1913E-3 -27 76 -55 37 -33 08 20 1674 J ^ 1 3 26E-9 3 5570E-8 1 1856E-2 4 1532E-3 -26 55 -65 86 -39 55 22 USADA 0347 M^ g <■ n f I 'i U.! n u N in 1 1 z •c £: ■n n ij r. a 4J o (11 o T, 1-H Q rr 1 II n m rf c "H m ^ 01 ■D r- c ^ ■H n r- 01 n T c m r~ •A r-f u ■^ m 10 n ^ M ^ in n [u o ii. ^ m ^ ■■0 H q. r~ n I- q- w ^ ul 1 ■B in a\ O tn 01 «f O Oi y Ol IQ Q r-j N fsi CTN r- r~ •n D D O O USADA 0348 MZ L' I i r. I r""- r I L- r u Ima GC 1.B7-2 - Manual DP File Edit View Calculate Report Parameters Status Help Data Filename : DAT A_On Folder ; 040806 Date : 04/08/06 Time : 17:48:39 Comment : 1 78/07 995474 F3l45uL ini 2uL : Parameters Automatic DP Params D o Data Prot^ssing Main Graph Graph Cursor Lines Window e.ooE-9- 6.D0E-9- < 4.00E-9- 2.00E-9- O.0OE-rt> -33.15 :m^7 -28.79 .-3i,aB ''-^■^^■'^ , \} , \\ , \ I il|i ' "l I . . Mil ' "" i . n irrrT D tuiapr n 200 400 600 800 iOOO 1200 1400 1600 1800 2000 Sees ri""''"iii(p 2200 2400 Li USADA 0349 ^10 Data Processing Results \ Data File Name : DATA Oil J- Folder : 04080e ' ' Sample Name : 178/07 995474 F3/45uL inj r '■ Sample ID J Sample Position 4 s 1 Injection Size 0. 0000 N , Sample Type Sam Method M-AN-41 ; S r Batch Name ] RunTime User micromass ' '^ Acquisition Time 17:48:39 Date : 04/08/06 V ^ Current Time 08:54:31 Date ; 05/08/06 N L^ r Analysis of Reference Gas Data I Ref Delta 13 = -34.50 Ref Delta 18 = -19.30 p- Time Major Ratio 2/1 Ratio 3/1 122 .7 8 .455E-8 1.1772E-2 4.2501E-3 ^- 182.7 8 .465E-8 1.1771E-2 4.2504E-3 242 .7 r 2423.5 8 .459E-8 1.1771E-2 4 .2502E-3 8 450E-8 1.1772E-2 4.2501E-3 ^ 2483.6 8 436E-8 1.1772E-2 4.2501E-3 2533.5 1 1 8 541E-8 1.1772E-2 4.2506E-3 'Std Dev Of Fit 3.1407E-7 ! 2 .2560E-7 Analysis of Sample Peaks, with Background Subtraction C02 ^ Time 79 7.1 p. 839.1 \ 871.9 '-- 88 0.6 909.0 ! L318.2 L1352.4 1671.2 Height Area 2/1 3/1 dC13Pk dC13Ekd dOlSPk d018 1.84E-9 1.7724E-8 1.1857E-2 4.2650E-3 1.63E-9 9.1742E-9 1.1778E-2 4.2295E-3 4.08E-9 1.7193E-8 1.1816E-2 4.1820E-3 4.07E-9 2.2454E-S 1.1841E-2 4.1969E-3 3.27E-9 2.5928E-8 1.1785E-2 4.2250E-3 4.22E-9 3.9586E-8 1.1830E-2 4.1764E-3 2.33E-9 2.1502E-8 1.1796E-2 4.1861E-3 2.57E-9 2.9485E-8 1.1859E-2 4.1584E-3 -27.16 -33 .77 -30.11 -28.04 -33.15 -28.79 ■31.88 ■26.16 -59.49 -59.43 -59.39 -59.16 -58.98 -57.10 -56.94 -55.38 -15.91 -24.09 -35.07 -31.63 -25.14 -36.38 -34.13 -40.52 9 9 9 9 12 12 14 n US AD A 0350 J^-L i.,' r: r- L.: r , 1 Li LNDD ENREGISTREMENT Codification : E-FCR-06 Version : E Date :24/l 1/05 I Page : 1/2 FICHE D'ANALYSE / RESULTATS GC/C/IRMS Echantillon : Repertoire: 178/07 B995474 040806 Instrument : GC/C/IRMS Isoprime 1 CO et paraphe: |26oV Valeur isotopique du reactif de derivation: ■53 Fraction Fl (metabolites de la cortisone et du Cortisol) Blanc urinaire Echantillon SI 1 1 Kfitoitio SI 1 1 Kfito^io Norn du fichier data 012 data 012 data 013 data_013 tr(s) 870 1490 870 1490 trr , 1.7U - 1.712 Intensite (nA) 2.0 2.9 2.9 2.7 5 '^C %o raesurfie -30.45 -24.56 -31,08 -24.75 5 ''C %a con-igee ■ -21.57 - -21.78 Fraction F2 fKetos) Nom du fichier tr{s) tn- Intensity (nA) 5 '^C %« mesuree 5 C %> corrig6e Blanc urlnaire SI data 014 869 2.4 -30.47 Etio data 014 1241 1.428 3.1 -25,54 -22.65 Andro data 014 1268 1.459 3.5 -24.63 -21.64 Echantillon Si data 015 870 3.5 -30.00 Etio data 015 1241 1.426 4.0 -26.58 -23.80 Andro data 0!S 1267 1.456 2.9 -27.93 -25.29 J Fraction F3 fDiols) Blanc urinaire SI 5P Adiol 5a Adiol 5(3 Pdiol Nom du fichier data_010 data 010 data 010 data 010 tr(s) 872 1323 1354 1 1674 trr . 1.517 1.552 L919 Intensite (nA) 5.3 7.0 2.0 3.3 5 '^C%o mesuree -31.54 -27,54 -28.31 -26.55 S'^C%(iC0iTig6e - -22.18 -23.11 -21.51 Echa ntillon SI 5p Adiol 5a Adiol 50 Pdiol Nom du fichier data Oil data Oil data Oil data Oil tr(s) 872 1318 1352 1671 trr - 1-512 1.551 1.917 Intensity (nA) 4.1 4,2 2.3 2.6 5 "C%o mesuree -30.11 •28.79 -31.88 -26.16 S'^CWocorrigee - -23,69 -27.43 -21.05 USADA0351 M. LNDD ENREGISTREMENT Codification : E-FCR-06 Version : E Date: 24/1 1/05 Page : 2/2 FICHE D'ANALYSE / RESULT ATS GC/C/IRMS 1 .; r u valeur de reference d'une population temoin Echantillon dans les normes 5 "C %<. haute 6 '^C %o basse oui non 1 1 Ketoetio -17.58 -26.27 < Etio -19.56 -26.10 « Andro -18.43 -25.02 o( Sp Adioi -18.55 -26.97 0^ SaAdioI -18.59 -27.40 V 5[3 Pdioi -18.25 -25.55 » f! l! 1 ; U r L L.. r i ■ (■ I J L: Blu Echantillon A%« A%o + 0,8%o A%. A%o - 0,8%o Etio - 1 1 Ketoetio -1.08 -1.22 -2.02 -2.82 Andro - 1 1 Ketoetio -0.08 -2.71 -3.S1 -4.31 5pAdiol-5pPdiol -0.67 -1.85 -2.65 -3.45 5aAdiol-5pPdiol -1.60 -5.59 '639 -7.19 Seuil de positivite de I'AMA : 6'^C%o(inetabolite) - 5 C%o(compose endogene de reference) > 3%o S'^C du compose < -28%o Variation maximale admissible liee a la methode: +/- 0,8%o Conclusion L'analyse par spectrometrie de masse de rapport isotopique indique une engine exogene des metabolites de la testosterone, coherente avec une prise de testosterone ou de I'un de ses precurseurs. L'origine exogene des metabolites de la testosterone a ete objectivee sur la base d'un appauvrissement isotopique de 3.51%o et -6.39%o respectivement pour les metabolites androsterone et 5a androstanediol. lj U Paraphe du responsable Observations: Partie a remplirpar le responsable USADA 0352 Ecart(s) n" : Cel enregistrement est a meltre dans le dossier de confirmation J55 LNDD EKREGISTREMENT Codification : E-CC-10 VK'sion; C Date : 09/05/2006 1/2 VERIFICATION DES PERFORMANCES INSTRUMENTALES EN CONFIRMATION CG/C/IRMS "««Anun Numerod'echantiUoii:..^'fe'ij?t. £fi3Si:^.5:^ Numiro d 'identification de I'appareil :„,.[.^,i;ai.j:i£.X Instruction de confirmation : ■Xcssw.f...'?'.) L! n L- U.' n !_> 1. Tune Sp&ification : plateau du peack Centre > 10 V Tunc conforme : oui 0^ non 2. Stabilite de I'lnstrnnient Specification: fcatt mesure entrc valeur maximale et valeur minimale du ratio 2/1 < 0.5 Ko Stabilite conforme : om non 3. Precision de rinstnimeiif Code de la solution Mix Cai HUMS: e:f?2v. Valenrs obt ennes f96o>Donr 3 ln| ecHi»tts; Decane Und^cane Doddcane M6thyld6canoate Moyenne -yi.yi -ai.Tt ->i.f6 -lf\-hl Ecart-type 0.£51- o,u o.lO o.tO specification: ecart-type d'au moins 3 alcanes < 0.5 %o Precision conforme : QUI O^ non L- USADA 0353 Jlij LNDD ENREGISTREMENT Codification; E-CC-10 Version : C Date: 09/05/2006 2/2 VERIFICATION DES PERFORMANCES INSTRUMENTALES EN CONFIRMATION CG/C/IRMS L n r-. I i u n L.J D I ■ 4. CalibratJon de I'instniment Code de la solution Mix Cal Acita.U:..,fr^?k.'^. Valeiirs obtenaes (%o ): 5a Androstaool AC Etiocholanblonc AC 5b Aadrostanediol diAC 1 1 Kitoetiocholanolone AC d,AA^.W=fS -■i=.kci — (?.s-? - as.n - (t-'YM d><:&\/« .•=Jl& -■fe.-Lr - (S.-^r- - yh.Q.2 ~\C.<^? Intervalle de valeurs acceptables: 5a Andiostasol AC Etiocbolanoloiie AC Sb Androstancdio! diAC 1 1 Kftoetiocholaiiolone AC Valeurs thforiques -30.46 -19.91 -33.81 -16.30 Vaicurs thfe)riqucs + 0.5%o -29.96 -19.41 -33.31 -15.80 Valeurs thferiques - 0.5%o -30.96 -20.41 -34.31 -16.80 Resultats confonnes : oui non Observations: Resultats : CONFORME / NON CQfilFQRME Raycr la mention inutile Vafidatioa Op^ratear Respoosable Date Code ct Visa Date Code et Visa ^(l?l& ^of oS\o%,\cilS SS VftLir, "VV \ Cet enregistrement est d trammettre au responsable du secteur corfirmation concemi puis A archiver vhianl dans le dossier matiriel de ['appareil concern^ dans la section correspondante. USADA 0354 J^ r ■■- i 1 LI n u n u n r "i iJ f ) i^ s%Uin8GC:liB7-2 Inlet Mass Spec Scan Jests Analysis User program Config Hetp .Current Mass : 45.00 Date .04/08/06 time :10:"21:2? "'" ■" ""' Mass-44 = 4.6664E-9 A Mass-45 = 5.4958E-11 A tvlass-4G = 2-0058E-n A FID =0.11610 V vScian^Display Window Graph Cursor Lines Window Scan 4.60E-3- 4.40E-3-; <4.£0E-3, Srce status = Penning = 2.8E-GmBat Pifani = 1.4E-2mBaf Turbo speed= 1.0E+2mBar 4,00E-3- 3540 fi.OE-9. 6.0E-9-i £ 4.i:iE-9- < 2.0E-9. I J I I I 3540 354£ 3550 3555 3560 " -I 1 1 1 I M 3565 3670 I AV " ini :□ 146/ Us/ 3575 35S0 3565 3590 3595 ^ 3545 3550 •"•'' I ' ' I 3555 3660 3565 3570 I'.'i/ 144 l45 i46 3575 3580 35S5 3590 3S95 USADA 0355 JH Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position Injection Size Sample Type Method Batch Name RunTime User Acquisition Time Current Time DATA 05 040806 Stabilite 5 1 0-0000 Sam C02-STAB 040806 micromass 11:08:45 Date 11:19:48 Date : 04/08/06 04/08/06 l^ Ui I) n „ ^ Analysis of Reference Gas Data Ref Delta 13 = -34.50 Ref Delta 18 = -19.30 Time Major Ratio 2/1 Ratio 3/1 42 .5 8-495E-8 1.1779E-2 4 .2534E-3 102.5 8 .499E-8 1.1779E-2 4.2535E-3 162 . 6 S.506E-8 1.1779E-2 4 .2539E-3 222.6 8 .502E-8 1.1779E-2 4 .2538E-3 282 . S 8 .494E-8 1.1779E-2 4 .2542E-3 342 . 6 8.489E-8 1.1779E--2 4.2543E-3 402 .6 8 .451E-8 1.1779E-2 4.2542E-3 462 . 7 8 .487E-8 1.1779E-2 4.2543E-3 522 . 7 8.458E-8 1. 1779E-2 4 .2540E-3 582. 7 8.439E-S 1.1779E-2 4.2538E-3 ..Std Dev Of Pit 1.7272E-7 2.7766E-7 U Analysis of Sample Peaks, with Zero Subtraction rc02 J Time Height Area 2/1 3/I dC13Pk dOl8Pk r ''■ USADA 0356 M Data Processing Results Data File Name : DATA 006 Folder : 040806 Sample Name : Mix Cal IRMS 003-1 Sample ID Sample Position 1 Injection Size 0.0000 Sample Type Sam Method M-AN-38 Batch Name 040806 RunTime User micromass Acquisition Time 11:30 r 41 Date : 04/08/06 Current Time 11:46:25 Date : 04/08/06 j i Analysis of Reference Gas Data L.' Ref Delta 13 = -34.50 Ref Delta 18 = -19.30 u Time 42.6 102.6 742.8 802.9 8 8 8 8 Major 498E-8 503E-8 421E-8 412E-8 Ratio 2/1 1.1778E-2 1.1778E-2 1.1777E-2 1. 1776E-2 Ratio 3/1 4.2537E-3 4.2534E-3 4.2519E-3 4.2519E-3 d Dev Of Fit 1.2485E-7 1.0555E-7 Analysis of Sample Peaks, with Zero Subtraction IC02 Time Height Area 2/1 3/1 dC13Pk dOlSPk I •- 191.6 5.57E-9 1.4452E-8 1.1796E-2 4.17a6E-3 -32.30 -36.54 i--! 259.1 4.36E-9 1.2956E-8 1.1B4SE-2 4.1803E-3 -27.78 -36 13 350. 9 4.90E-9 1.4134E-8 1.1801E-2 4.1745E-3 -31.79 -37 39 p 538.2 5.18E-9 1.4106E-8 1.1805E-2 4.1624E-3 -31.30 -40 09 ■U u USADA 0357 jn Data Processing Results Data File Name : DATA 007 Folder ; 040806 Sample Name Mix Cal IRMS 003 -2 Sample ID Sample Position 1 Injection Size 0.0000 Sample Type Sam Method M-AK-38 Batch Name 040806 RunTime User micromass Acquisition Time 11:46:27 Date : 04/08/06 Current Time : 12:06:32 Date : 04/08/05 Li „ ^ Analysis of Reference Gas Data Ref Delta 13 = -34.50 Ref Delta 18 = Time 42.5 102.6 742 . 8 802.8 -19.30 Major 8 .470E-8 8.526E-8 8.343E-8 8. 391E-8 Ratio 2/1 1.1776E-2 1.1777E-2 1.1777E-2 1.1776E-2 Ratio 3/1 4.2S27E-3 4.2529E-3 4.2518E-3 4 .2516E-3 4 .2211E-7 1.2081E-7 : Std Dev Of Fit U Analysis of Sample Peaks, with Zero Subtraction ! :C02 Time Height Area 2/1 3/1 dCl3Pk dOlBPk lyi 1 3 77E -9 257 4 2 88E -9 349 8 3 23E- -9 536 7 3 50E- 9 8.8306E-9 1.17g3E-2 4.1702E-3 7.8902E-9 1.1844E-2 4.1722E-3 8.7038E-9 1.179aE-2 4.1711E-3 8.2134E-9 1.1803E-2 4.1643E-3 -32.44 -27.99 -31.93 -31.44 -38.33 -37.85 -38.05 -39.56 r L 1' L. USADA 0358 JSOi Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position Injection Size Sample Type Method Batch Name RunTime User Acquisition Time Current Time DATA_0 08 040806 Mix Cal IRMS 03-3 1 0. 0000 Sam M-AN-3S 040806 microraass 12:02:11 Date 12 :21:06 Date 04/08/06 04/08/06 .e. .eua X3 =-^^-f|.- -r— ---_^^^^^ Time 42.5 102.6 742.8 803.1 Major 8.462E-e 8. 517E-8 e.365E-e 8.370E-8 Ratio 2/1 1.1776E-2 1.177eE-2 1.1777E-2 1.1776E-2 Ratio 3/1 4.2524E-3 4.2526E-3 4.2519E-3 4.2520E-3 4 .2009E-7 i Std Dev Of Fit ^ Analysis of Sample Peaks, with Zero Subtracti rico2 - Time Height Area 2/1 1.8134E-7 on 3/1 dC13Pk 191.1 d018Pk 349.8 [■-;, 536 . 8 5.46E-9 ^ «— 1.3084E-8 1.1799E-2 4"i708E-3 1.2814E-8 1.1806E-2 4.1655E-3 -3^:22 -27.81 -31.60 -38.56 -38.09 -38.12 -39.31 ;-j 1 ; USADA 0359 J30 Data Processing Results Data File Name Folder Sample Name Sample ID Sample Position Injection Size Sample Type Method Batch Name RunTime User Acquisition Time Current Time DATA 09 040806 Mix Cal Acetate OOlA-lOOng inj 2 0.0000 Sam M-AK-41 micromass 12:24:14 Date 04/08/06 13;45:11 Date 04/08/06 Analysis of Reference Gas Data Ref Delta 13 = -34.50 Ref Delta 18 = -19.30 Time Major Ratio 2/1 Ratio 3/1 122.5 8 .507E-8 1.1776E-2 4.2528E-3 182.6 8 .550E-8 1.1776E-2 4.2528E-3 242.6 8 493E-8 1. 1776E-2 4.2530E-3 2423 .4 8 .422E-8 1.1775E-2 4.2523E-3 2483.5 8 354E-8 1 .1775E-2 4.2518E-3 2533 . 5 8 443E-8 1.1775E-2 4.2521E-3 td Dev Of Fit 9.2732E-8 1.7392E-7 Analysis of Sample Peaks, with Background Subtraction CO 2 Time Height Area 2/1 3/1 dC13Pk dC13Bkd dOlSPk dOia 870.6 4.30E-9 2.0644E-8 1.1815E-2 ,. 1241.8 4.36E-9 3.5212E-8 1.1934E-2 I 1316.7 3.35E-9 2.6894E-8 1.1777E-2 L- 1491.1 2.83E-9 3.1S04E-8 1.1971E-2 4 1628E-3 -30 40 -76 48 -40 04 32 4 1653E-3 -19 98 -74 28 -39 4S 31 4 1662E-3 -33 71 -74 11 -39 21 31 4 1687E-3 -16 74 -74 00 -38 66 31 I ", i I L-v' USADA 0360 ^A L.' r I . I i u i 1 u l^ 1 : f ! L- f ■ File Edit View Calculate Report Param'SS^SII^SJ Dala Filename : DATA,D09 Folder ': 04O80S Date :04^08iOG Time :1224'14 Comment : MwCalAcetateOOtA-lOOngini Paiamelers Automatic DP Params Graph Cursor Lines Window LOOE-S, e.ooE-&- 6,00E-9- < 4.00E-S- 2,00£-9- O-OOE+O ^-30.40 ,-■19.98 *■ u -33.71 ,-.-lS.74 , ^ i"' ''i' !r7f . )T7T £00 400 600 eOO 1000 1200 ° IDI ° D 1200^ 1400 1600 1600 2000 2200 2400 IfiBaor !"■ L US AD A 0361 Jil Data File Name Folder Sample Name Sample id Sample Position Injection size Sample Type Method Batch Name RunTime User Acquisition Time Current Time Data Processing Results DATA_016 040806 Mix Cal Acetate OOlA-loOng inj 9 0.0000 Sam M-AN-41 microraass 07-33:19 nif^ ■■ OVO8/O6 ^'.Ji.l9 Date : 05/08/06 Kef Delta 13 .^^^^^3^! of Reference Gas Data ■i^.bo Ref Delta I8 = n J ri L; Time 122.5 182.6 242. 5 2423.4 2483.4 2533.5 Major 8.534E-8 8.513E-8 B.502E-8 8.433E-S 8,404E-8 8-484E~8 -19.30 '^Std Dev Of Fit n Ratio 2/1 1.1775E-2 1-1775E-2 1.1774E-2 1.1774E-2 1.1774E-2 1.1773E-2 4.6118E-7 Ratio 3/1 4.2534E-3 4.2533E-3 4.2532E-3 4.2522E-3 4 .2518E-3 4.2521E-3 1.1639E-7 C02 r'i Time '^' 870.5 ,,.,1241.6 ■ 11316.1 U149O.4 u --.-s o. s.„p.. ,..,., „,,, ,^^^^^^^^^ ^^^^;^^^^^^ Height Area 2/1 4 .31E-9 4.22E-9 3.28E-9 2.97E-9 1.9411E-8 1.18I5E-2 3.4868E-8 1.1933E-2 2.7273E^8 1.1777E-2 3.0767E-8 1.1970E-2 3/1 4.1647E-3 4.1679E-3 4.169SE-3 4 .1690E-3 dC13Pk_dC13Ekd dOlSPk d018 -30.25 -19.95 -33.63 -16.58 -79.02 -77.2 9 -77.27 -77.62 -39.67 -38.91 -38.50 -38.62 34 33 32 32 U w I I u ( : USADA 0362 yi33 r: r- u D D n r -I U Fife hdil View cSX Repor^SS^^S^^ Das. Fiienafne:DATA_016 lolder : ^OEoI " Date : 04^08/06 j-^^ ,21.32.21 Comment : Mix CalAcetate OOlA-1 OOng ini Parameters Automatic DP Pajams Graph Cursor Lines Window S.OOE.Q ° \a\ 6.00 E* E < n 4.00E-9 £,0OEe- 0,CiOE+o: WW J^ I I II I fr >-30.25 ^.i9_35 ^ ^ ' IT T *-='"^16M £00 400 600 eOO 1000 " D ~ M I . I I^ x. llulainr ^12° ^'^°° ^500 1800 2000 2200 2400 u u USADA 0363 Ji^ INQ) cofrac LAB0»AT011?E NATIONAL DE PtflSTAQF DU OOPAGF ■l%h r ,■ !_■ t r u Chatenay-Malabry, le 05 aoQl 2006 ESsTlTs ACalDITUION r, H*i-ii7* Li . ' *> R APPrn^T HE rONTRF, ANALYSE ,J^^, SU« DENUWDE D«nfl«d« de confre-ana/j'sc dc I'UCI et de VUSADA du SljuiUet 2006 suite au rapport d'amlyse n°178/07-l ^ Prelevements du Dr. BORDABERRY Organisme : CycLisme (UCI) Epreuve et lieu : TDF 2006 : 17'°* etape a MORZINE Date : 20/07/2006 Reception defsl l'echantillonfs> d'urine : Date : 20/07/2006 Type de materiel : Berlinger Nombre d'echanlillon(s) : 1 ( sur 3 ichantillons re?us) Reference de(s) l'tehantillon(s) : I78/07_995474 B Resukais {Cf referenOels en vigaeur : AMA / ReglemerOation nationaU - contrSle en Competition) Date de debut des analyses : 03/08/2006 ^' M^tfaodes utilise : Chromatographie gazeuse couplee k la spectrorndtrie de masse GC/MS (EC24D) et r Spectrom^trie de masse de rapport isotopiciue GC/C/IRMS (EC3 1 ) r: conclii^nii (pH=5.2 d=L025 +/-0.002) L; T/F.p : r L'origine exogene des metabolites de la Testosterone a ete objectivee sur la base djmi appauvrissement isotopique de 6.4 -Kk, et 3.5 %o, r^spectivement pour les metabolites 5a-AndrostanedioI et Androsterone. Rfisultat expriP^^ p«r rapport g" ''■^nil de nositivJte de TAMA : . Appauvrissement isotopique > a 3 %o (variation maximale admissible appliquee au laboratoire = 0.8%o) 1—1 ) i i_- r; r ■ : Union Cydiste Internationale - C. VARIN (CH 1860 AIGLE - SUISSE - President du Conseil de Privention et de Lutte contre le Dopage (39 rue St Dominique- 7570U KAKis; Pour information : sous M forme incigrale. (I est confidentiel el comporte 2 page(s). ^ '^M USADA 0366 •-^ l_l U: u L, B-sample analysis 995474 Firth of August 2006 Chatenay-Malabry Statement no. 1 As an expert Dr. Douwe de Boer has been witnessing in the period between August 3 and August 5, 2006, the B-sample analysis in the LNDD, the WADA- accredited anti-doping laboratory in Chatenay-Malabry. Statement no. 2 The impression of the expert regarding the analytical perfomiance of the B-sample analysis was that the LNDD worked in a transparent and professionnal way and according to transparent and professional procedures. Statement no. 3 U I" f In respect to the semi-quantitation of the ratio between testosterone and epitestosterone (TIE ratio) as well as of the concentration of testosterone and epitestosterone it must be stated the following: A) A ratio was established between two peaks in the chromatogram. B) The identity of the compound(s) belonging to the peaks has not been established according to the minimal WADA requirements. Therefore, any official conclusion regarding to the T/E ratio as well as of the concentration of testosterone and epitestosterone is and will be premature. As such any ofncial conclusion in relation to the above mentioned parameters of the respective sample is non-conclusive. J3>1 USADA 0368 statement no. 4 r'r n In respect to the GC/C/IRMS analysis it must be stated the following: A) During the B-sample analysis it was not possible to see documentation and data regarding the uncertainty of the GC/C/IRMS analysis, which was reported to be 0.8%o. B) During the B-sample analysis it was not possible to see documentation and data regarding the historical data of blank urine pool no. 4. Therefore, it was for the expert not possible to give an adequate evaluation of GC/C/IRMS analysis of the respective sample. The above mentioned issues have been implemented into a list of requests addressed to Prof, de Ceaurriz. U Or Douwe de Boer LJ n D 1-1 I I u L L USADA 0369 MS INED LABOBATOIKE NATIONAL DE PEPlSTACE DU DOPAGG List of the requests from Dr. Douwe de Boer Counter-analysis on "B" 995474 > The GC/C/IRMS has been accreditated by the WADA and the French National Accreditation body. Would it be possible to see the documentation regarding this accreditation? If so, I would appreciate to see the documentation regarding the accreditation. r. i Lv r'" Li > In principal a WADA accreditated laboratory is participating in proficiency programs. Would it be possible to see data of the Chatenay-Malabry laboratory? If so, I would appreciate to see the data regarding the GC/C/IRMS analysis. [! I' I ■ L. L > The certificate of the analysis of the A-sampIe mentions an "uncertainty" of 0,8%o for the GC/C/IRMS result. Would it be possible to see documentation and data of how this value of "uncertainty" was established? If so, I would appreciate to see documents and data regarding the establishment of the value of 0,8!6a. > Historical data regarding the blank urine pool no.4, which has been used in the GC/C/IRMS procedure. Would it be possible to see documentation and data regarding the history of blank urine pool no.4. If so, I would appreciate to see the repeatability (intra-day variation) and the reproducibility (inter-day variation), meaning the average value, the standard deviation and the number of observations made. lousve de Boer Pr. De CejMirriz 143, avenue Roger Salengro - 92290 Chatenay-Malabry - FRANCE j og Telephone : + 33 (0)1 46 60 28 69 - Telecopie : +33 (0)1 46 60 30 17 ■ e-mail : dLrection@lndd.com ^^ USADA 0370