BOOK --~N~O~~:l_l_7_81
`J?l.fJVAr/111/ tile h-ee, D .00'1%
`TITLE
`
`fVr,.. .. t(,"WI< /p, f&T
`
`PAGE~-~N~0~:~1~9 __
`PROJECT#_:_)_?_S"7~/f~~~-
`
`,,
`o.ooVZ
`
`Exoerimental:
`
`Egumment:
`Mettler AX 205 DR Analytical Balance, Asset No. 515840, Rm. Bl34 (referred to as Balance 1)
`Mettler PG 5002 Balance, Asset No. I 0 I 265, Rm. B 134 (referred to as Balance 2)
`Orion 525A+ pH Meter, Asset No. A2309, Rm. Bl 34
`The Advanced Micro-Osmometer Model 3300, Asset no. 00103390, Rm. Bl 32
`Stir Plates, Rm. BI 34
`Millipore 0.22 µm Filter Unit (IOOO mL)
`
`Formulations:
`FID
`Batch
`109032
`05-40452
`109033
`05-40453
`109034
`05-40454
`
`Description
`TRA VAT AN BAC Free, 0.004% - pH 5.5
`TRA VAT AN BAC Free, 0.004% - pH 6.5
`TRAVATAN BAC Free, 0.004% - pH 5.5 w/ 85% of zinc, boric acid
`
`---- r:.••;:n;O::::•d••:,:::• 0:::: b::A::~:i::~j::~::·::: _pH 55
`h~ I Tare weighed a clean glass beaker·with a stir bar. (Balance 2) tf> t;,,...,,-
`. -~-,.
`/ 2: Removed the stir bar. Weighed and added the batch quantity ofHC0-40 directly in the beaker.
`(Balance 2) M ~--3;i,-
`'
`_4.o'1 3. Added about 5V % of batch quantity of purified water. fr°; f-~·"'7
`·fl'
`4. Stirred for at least 15 minutes until HC0-40 is dissolved. M >-J-t>,--
`5. Weighed and added the batch quantity of the following excipients to the beaker: boric acid,
`sorbitol, propylene glycol, and zinc chloride. Stirred the solution to dissolve these ingredients .
`(Balance 1) IX ->/~_,,,.,
`·
`6. QSed to 95% of batch weight with purified water. (Balance 2) tb'>-·N?
`Initial pH= '(. cJ/()
`,~ P-l~r-
`7. Measured the pH.
`8. Adjusted pH ifnecessary.
`Amount of IN HCL added= 11)11'1
`Amount of 1 N NaOH added= (}. 'f{Jf
`
`flr;}--i·()S·
`
`If:"("- i?-17~
`9. Weighed the batch quantity of AL-0622 I using a spatula. (Balance 1)
`The spatula was placed in the bottle with the end containing AL-06221 immersed in the solution .
`I 0. Covered the opening with parafilm to minimize evaporation. Stirred overnight to dissolve the AL-
`06221 .
`r1r >-J--o>
`Stirring Start time and date: S: IS It'-
`.lls' ~-fc,,-
`StirringStoptimeanddate: 1:1lO """'
`11. QSed to 100% ofbatch weight with purified water. {Balance 2) Final pH= .5.--. s)f If) 5-'l"t?
`12. MeasuredOsmolality. Osmolality= ;J<t'? .... 0-s~/I; tk 5-'fo1
`
`• • • • • • • • • • • 1• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • •
`
`ADJUNcr1vE DATA ~ ,_~ ,..,~
`'1 fllf /')
`PAGE
`bAJ 1178 I. If
`REF
`
`Verified By :
`&~1111-
`
`CONFIDENTIAL – PROTECTIVE ORDER MATERIAL
`
`(cont. on page _~_O __
`
`Date
`b-)-1-c?~
`
`ALCON 2009
`Argentum Pharm. LLC v. Alcon Research, Ltd.
`Case IPR2017-01053
`
`

`

`NO: 11781
`BOOK
`T~ltl!A77W Mc F;.ee, o.ouY'l1
`TITLE
`(cont. from pag::. _ --+l+1--
`
`fvr"""'~k;t( '1r IE r
`
`PAGE
`PROJECT#
`
`NO: 20
`;}'l Dlf
`
`B. FID 109033
`
`Batch 05-40453 TRAVAT AN BAC Free, 0.004% - pH 6.5
`
`I. Tare weighed a clean glass beaker with a stir bar. (Balance 2) /If f- ~..,,~
`2. Removed the stir bar. Weighed and added the batch quantity of HC0-40 directly in the beaker.
`(Balance 2) ~ ~-:i·~1
`3. Added about 5'0 % of batch quantity of purified water. "55+.:>>
`4. Stirred for at least 15 minutes until HC0-40 is dissolved. tk !f'-J·o'f
`5. Weighed and added the batch quantity of the following excipients to the beaker: boric acid,
`sorbitol, propylene glycol, and zinc chloride. Stirred the solution to dissolve these ingredients .
`(Balance I)~ (·]-oif
`6. QSed to 95% of batch weight with purified water. (Balance 2)/'t; ,--J-tJS
`Initial pH= ~· 0'7l, ~ 5>J.at;
`7. Measured the pH.
`A7 r- 'j-Qf.'
`
`, J Adjusted pH ifnecessary.
`
`Miff/
`Amount of IN HCL added= iv
`Amount of IN NaOH added= f. lf11
`
`1
`(/
`
`Weighed the batch quantity of AL-06221 using a spatula. (Balance I) ~ s-:J-o::>
`The spatula was placed in the bottle with the end containing AL-06221 immersed in the solution .
`I 0. Covered the opening with parafilm to minimize evaporation. Stirred overnight to dissolve the AL-
`06221.
`'3: ''f"' A-s }-$·C?
`Stirring Start time and date:
`(,.S5 3 @j)~ ~-r.,,,.
`Stirring Stop time and date: q:DOA,.. M 5-t/.o5
`11. QSed to I 00% of batch weight with purified water. (Balance 2) Final pH= I ;;i!1 uc6L1~ ¢t ,_
`12. Measured Osmolality. Osmolality = 'J ?g mO~,.. /ieJ
`14-r 5-f-"7
`
`C. FID 109034
`
`Batch 05-40454 TRA VAT AN BAC Free, 0.004% - pH 5.5 w/ 85% ofzmc,
`boric acid
`
`1. Tare weighed a clean glass beaker with a stir bar. (Balance 2) If< ./'-~'T)'
`2. Removed the stir bar. Weighed and added the batch quantity of HC0-40 directly in the beaker.
`(Balance 2) ~ t--?-c~
`7
`3. Added about 5lJ % of batch quantity of purified water. "" r
`7P>
`4. Stirred for at least 15 minutes until HC0-40 is dissolved. IH ~j,,;,<;
`5. Weighed and added the batch quantity of the following excipients to the beaker: boric acid,
`sorbitol, propylene glycol, and zinc chloride. Stirred the solution to dissolve these ingredients .
`(Balance I) fi'k ?~ -o<;
`QSed to 95% of batch weight with purified water. (Balance 2) & 5-s-o~
`Measured the pH. Initial pH= lf.J~? M ~-~-Ps
`Adjusted pH ifnecessary.
`A
`Amount of 1 N HCL added= IJ/n
`Amount of 1 N NaOH added= t). ??f If~ ~-iN~
`
`6 .
`
`7 . r irJ
`
`;y;~.
`
`···~"·
`
`10 .
`
`r
`
`Weighed the batch quantity of AL-06221 using a spatula. (Balance I) ~ r::J..,,!i"
`The spatula was placed in the bottle with the end contaming AL-06221 immersed in the solution.
`Covered the opening with parafilm to minimize evaporation. Stirred overnight to dissolve the AL-
`06221.
`,
`d....
`""> >-'l""s
`'? · 15 ;,.,
`Stirring Start time and date:
`"1 t D iJ °" IJ1
`.
`,1- .r-'(-c->
`Stirring Stop time and date:
`11. QSed to I 00% of batch weight with purified water. (Balance 2) Final pH= S--. 'f' "Jf 7k ~-'(-c-S
`12. MeasuredOsmolahty. Osmolality= ;)t;-)""'Q,..(f_r IJ 5 .l-Y-os-
`' - - - -
`
`• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • •
`
`Verified By :
`1¢~'YCA
`
`Date
`c, ... ~....,,y
`
`Entered By :
`
`(cont. on page
`
`;J.. f . )
`
`Date
`6-J/'fls
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`

`

`BOOK
`NO: 11781
`TITLE TRAVArAN ~Ac Fr.ee , 0. ()P'f % Fvrl'll .. £ hv11 fi, tF1
`
`PAGE
`PROJECT#
`
`NO: 21
`'J-).~)/t
`
`·-··;_~-; ... R;;;;~·: ··;w ~- y~s
`f.tiL .. .!f/!2.d,,
`.(;;( ..
`
`...... , ... fr,1i-I
`
`€Pc/
`
`to.t.:
`
`ADJUNCTIVE DATA /kt->t~-·--·-·-···-·:·· .. --.
`/ f /lffr{
`PAGE .
`~-............ REF ... -·-·m· t-N ![)"fl'. )T··-·--
`
`. --··-··-···
`
`..
`
`__ jEr t(At"':~~~v"'_:~~-V-ilJ-
`_
`0)- V<J'(~ )-,(,, os--'{ut/n-1 , eiv/ Cs-
`. 5"/ .... :f hJff
`f£'[, .. tl~ f
`. U'!! L.{~!!::1l?J'.£-:-
`s IJ .~ .. Io oo d.~~F8
`
`-···-· ............ .
`Iv tn.cmt:v~ fbr .
`tjutfs'/-1
`............. ., .. , .................................. ., ..... .
`
`_/!11e.lb'tJ/.gfJwr5 / { (fOh'r~h) ' tk ~ ·£-~
`~:Iv fac/ ft,t. 1Pr,ft) :/fJ1,·cr(Jh10hfy
`.. lo. 4N<f!i'r.:./ ~JP>n,ifry tPr
`. ............... :~s. '>:"$..:;;;.<?.'I:.... . .......... .
`&vn't 4c.J l,ot ti>s-7
`2,~( ... 0 . oo~~j_ .. ~~fpt.
`
`'/
`
`/
`
`$1).i'lf'ie D t"
`
`·-·-........ --·-···-···--------···--·
`
`f/et/hw.>;:; k~I:
`
`• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • •
`
`. i;;r. f!~~~I~.:: .. ~(t!_ .. 6-~'· 0'i'
`lots {1--L,..,-o .. J l/;r (;;~v5/ ;11sr
`All
`. . !Ni 't? t1~ t!:!:J:li£.,. Ii:!;,.,•,,.,,.,.
`. 'fb!J1Ja1n;'i£ ... t((<-<(lf _' f{( /;-)JO~ .
`<{<e _(..0'.urc{,·v-f ~fc. hr c,/( tl/1er·y/c,,,/ Ck'?'r(/y hSe,J/) .
`
`us( 111t,'r:t',."t',..h:.
`
`{v,..17k iJ,,,;.Jk r--7tr.I
`
`Verified By :
`fb~17'1)-
`
`Date
`
`Entered By :
`
`' ... 2."1--r
`
`(~ont. on page plVJf. )
`
`Date
`ft? -). f -0 5,,-
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`