• •
`....
`
`•
`
`p~GE __ .:...;N"""O;.:__: 2....,1._-~\-
`NO: 10750
`BOOK
`i
`\..d :to.~~.
`/
`PROJECT #
`2.~lt 21 0
`TITLE {>{;T:u~~ AL-li~:ll o.od1?o ~Sdn1\crt el-l-3lt!oS-~ lf1t>IO!t039J
`
`. ,., • • • • • • • • • . , • • • • • •• ·(cid:173)• • • 1• • 1: 1: ••• ... •• • 1• 1• :e • • • ••
`
`CONFIDENTIAL – PROTECTIVE ORDER MATERIAL
`
`Date ~-fc Entered By ;
`~ ....U..U.~"-'
`
`. . - ' --r-----: --,-_.
`
`ALCON 2020
`Argentum Pharm. LLC v. Alcon Research, Ltd.
`Case IPR2017-01053
`
`
`....
`
`•
`
`p~GE __ .:...;N"""O;.:__: 2....,1._-~\-
`NO: 10750
`BOOK
`i
`\..d :to.~~.
`/
`PROJECT #
`2.~lt 21 0
`TITLE {>{;T:u~~ AL-li~:ll o.od1?o ~Sdn1\crt el-l-3lt!oS-~ lf1t>IO!t039J
`
`. ,., • • • • • • • • • . , • • • • • •• ·(cid:173)• • • 1• • 1: 1: ••• ... •• • 1• 1• :e • • • ••
`
`CONFIDENTIAL – PROTECTIVE ORDER MATERIAL
`
`Date ~-fc Entered By ;
`~ ....U..U.~"-'
`
`. . - ' --r-----: --,-_.
`
`ALCON 2020
`Argentum Pharm. LLC v. Alcon Research, Ltd.
`Case IPR2017-01053
`
`
`
`Alcari
`R&DLIMS
`
`\01 "S0~\-.2
`
`Formulation Report
`Page 1of1
`21·APR-2004 01 :28 PM
`
`Report Date:
`
`Vers. 2
`Formulation ID: 106039
`Description: AL6221 0.004% Oph. Soln. (Preservative Free)
`Dosage Form: SOLUTION
`Target pH: 6.0
`Units: WN %
`
`Component
`Al06221
`Polyoxyl 40 Hydrogenated Castor Oil
`Boric Acid
`Sorbitol
`Zinc Chloride
`Sodium Hydroxide
`Hydrochloric Acid
`Purified Water
`
`Concentration
`0.004%
`0.5%
`1%
`1%
`0.0025%
`adjust pH
`adjust pH
`q.s. 100%
`
`Purpose
`Active Ingredient
`Surfactant
`Buffering Agent
`Necessity
`Excipient
`Ph Adjust
`Ph Adjust
`Vehicle
`
`Database: LIMSAR
`
`FB_FonnRep_Short.02.LIMS037.0.01 2004.P0002250
`
`•
`
`•
`
`•
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`- - - - - - - - - - - - - - - - - - - - - - - -· ·--- -- .
`
`
`
`Product:
`Sample Tlmepoint:
`On Test:
`04/21/2004
`
`Notebook 10750
`
`Page 021· 3
`
`PRESERVATIVE RAW DATA
`
`Controls
`
`Initial
`
`Lot number:
`
`04/21/2004
`Date of Sample: - - - -- -- -
`Organism Counts at Dilutions
`
`10-1
`
`I
`~
`\
`\
`)
`I
`j
`\
`)
`(
`
`10-2
`
`/
`
`I
`
`\
`
`I
`
`""
`'
`\
`J
`I
`\
`I
`
`10·3
`
`/
`I
`l
`\
`
`""
`)
`I
`I
`\
`)
`(
`
`10·"
`
`IOI
`
`ID~
`-
`IOCS
`
`\ \CR
`
`\ \ ~
`
`\ '.l (')
`
`\ l') L\
`
`\ \ 'l.
`
`. -rklTf
`
`i~ TL
`
`10-~
`
`Plate Count
`Average
`
`Initials
`-Date
`
`\ l
`
`\ l\
`
`l~
`
`\ t)
`
`\0
`
`\S
`q
`I c:;
`
`\ ()
`
`l \
`
`~ · ~ -
`l\ I ~(p \ ot\
`t . J:l .
`4 b!Plo~
`~.lJ ,
`4 bu.\ott
`t.ll_
`41~10<1
`~ . .H_
`4 J~lt>lott
`
`(0
`\. D x \0
`
`ID
`I I 'it lO
`
`(;
`\.1. )( \0
`
`&
`\ \ ~\0
`
`"'
`\.I x \0
`
`Test Organism
`
`S. aureus
`ATCC 6538
`
`P. aeruginosa
`ATCC9027
`
`E. coli
`ATCC8739
`
`C. albicans
`ATCC 10231
`
`A. niger
`ATCC 16404
`
`MEDIA:
`
`•
`
`Peptone Lot (tubes):
`
`NIA
`
`_ Saline Lot (tubes): ott. 3~ ;is-I Polysallne Lot(tubes): Cll\ - 3<P~I
`
`MCTA Lot: O'-\Bo1S
`
`Polysallne ·Lot (bulk): ol\\\O:;l'-l
`Peptone Lot (bulk): __ N_IA _ _ Saline Lot (bulk): CL\\)01 (>
`Waterbath Asset No.:~~(l\oot~ Waterbath Temp(°C):
`Letheen Lot: .Q!l.:3u4 ~Lt - I
`Other: ___ J.J_l'-'--A- - -- -- - - ·- -- -·
`
`t..\5, lo
`
`ORGANISMS:
`
`A. niger Preparation Reference:
`
`Analyst: ~-~, Date:
`Verifled By:l{lZ~:.-:--:--~-. ---,-. - - Date:
`
`M40.02
`Rev. 10
`
`•
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Notebook 10750
`
`Page 021· L\
`
`PRESERVATIVE RAW DATA
`
`·•
`
`Product: AL-6221 0.004%0PH. SOLN.
`Sample Timepoint:
`Day 7
`On Test:
`04/21/2004
`
`Date of Sample: - -- -- - - -
`04/28/2004
`Organism Counts at Dilutions
`
`Lot number: 04-36405-2
`
`Test Organism
`
`10·'
`
`10-2
`
`\NTl
`
`\N\C..
`
`1'NTC
`
`\NTC.
`
`"l'~TC.
`
`°fNTl
`
`11
`
`1> 4a
`2.S
`32.
`
`211
`
`2'-i 0
`
`10·3
`
`\ \
`
`\~
`
`0
`3
`:1.2
`
`23
`
`S. aureus
`ATCC6538
`
`P. aeruginosa
`ATCC9027
`
`E. coli
`ATCC8739
`
`C. albicans
`ATCC 10231
`
`A. niger
`ATCC 16404
`
`MEDIA:
`
`10-4
`
`0
`
`\
`
`0
`
`0
`3
`'-\
`1y
`'"
`
`0
`
`1 o-'
`/
`I/
`/
`v
`/
`I/
`
`I
`'\
`
`0
`
`0
`
`Plate Count
`Average
`
`Initials
`-Date
`
`c . .tl.
`3 Sj3)ot.{
`i.o'IC \O
`t. . .ll.
`~13\oi.t
`e.1L
`~ l:~ \oq
`t . ..tL
`5 /s\ot\
`t..lL
`~ $/-s loL\
`l. 0 )( \O
`
`3
`l .C\ )( tD
`
`11
`2.3 x. \ 0
`
`5
`1.?x \O
`
`.,- N TC
`
`'TNTC..
`
`l°tJTl.
`
`\" N TC.
`
`INT(.
`
`INTC..
`
`'"T f\J'IC..
`
`"TN IC
`
`<i
`
`I~
`
`I
`
`2.
`
`-
`
`0
`
`....... . .
`
`Peptone Lot (tubes):
`
`NIA
`
`Saline Lot (tubes): O_q- ~ t,~l Polysallne Lot (tubes): OL\ -3~ \
`
`NIA
`Saline Lot (bulk):
`NIA
`Polysallne Lot (bulk):
`Peptone Lot (bulk):
`MCTA Lot: l\ OC\ \I.\ \.3._ Waterbath Asset No.:::\\,) (A ool ~) Waterbath Temp(°C):
`5 """\
`Letheen Lot: OY .. ~~ Oj.- \
`._""-'-\A~---------------
`
`Other:
`
`NIA
`
`ORGANISMS:
`
`A. nlger Preparation Reference: NIA
`
`Transfer Log Reference: NIA
`
`~-~------
`
`-~~~~-
`
`Analyst: _~~
`Date:
`Date: - l!flf U-
`Verified By: ~a,..:(e_dk ~
`
`M40.02
`Rev. 10
`
`•
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Notebook 10750
`
`Page 021- 5
`
`PRESERVATIVE RAW DATA
`
`•
`
`Product: AL-6221 0.004%0PH. SOLN.
`
`Lot number: 04-36405·2
`
`Sample Timepoint:
`On Test:
`04/21/2004
`
`Day 14
`Date of Sample: - - -- - - --
`05/05/2004
`
`Organism Counts at Dilutions
`
`Test Organism
`
`S. aureus
`ATCC 6538
`
`P. aerugi11osa
`ATCC9027
`
`E. coli
`ATCC8739
`
`C. albicans
`ATCC 10231
`
`A. niger
`ATCC 16404
`
`MEDIA:
`
`•
`
`10-'
`
`\ q
`
`.14
`
`2.
`3
`
`i"N\C.
`
`\ NT'C ..
`
`10·2
`
`~
`5
`
`0
`
`0
`5:;
`
`1~
`
`-rNTC
`
`'f /\J TC.
`
`-fNT(..
`
`,- Ni"c.-
`
`1' N \(.
`
`\ N \C..-
`
`~
`
`9
`
`10·3
`
`10-4
`
`10·'
`
`/
`/
`
`'f"NTC
`
`~;
`
`\NTL
`
`/
`
`/
`
`/
`/
`/
`I/ /
`/
`·/
`/
`/
`/ v
`/
`/
`/
`/
`/
`I/
`/
`
`/
`
`/
`
`0.4
`
`/
`
`/
`
`Plate Count
`Average
`
`I
`
`.2.5 x \C>
`
`Initials
`-Date
`~ . ;.
`~ 5l\o (oq
`2.2.X \ 0
`e .. lL
`5 !to lott
`t . .tl.
`3 ~ ltolo~
`l.. .1 x \ 0
`t.~ .
`5 SJ. ~lo~
`i. ~ )I \ 0
`t . .l:I,
`'I I :il-0'4
`
`l
`~Sxlo
`
`..
`
`Peptone Lot (tubes):
`
`NIA
`
`Saline Lot (tubes): CL\-3(o'S\C\ ·l Polysallne Lot (tubes): 04 ·3(1501-\
`
`N/A
`N/A
`Peptone Lot (bulk):
`Saline Lot (bulk):
`Polysallne Lot (bulk):
`- - - -
`-
`-
`-
`-
`MCTA Lot: '-\ OC\ \ l.\ \ C\ Waterbath Asset No.: ~~OOS~ Waterbath Temp(°C):
`l\ I.fl.\
`_...;.~---'-'-lA..__ _ _ _ ____ ____ _ _
`Letheen Lot: c4 - ~u~ <:\o .. \
`Other: _
`
`N/A
`
`ORGANISMS:
`
`A. nlger Preparation Reference : N/A
`- --------
`
`Transfer Log Reference: NIA
`--~~--
`
`Date:
`
`Date:
`
`M40.02
`Rev.10
`
`•
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`101'$0
`Page ~l- ~
`Notebook
`INVESTIGATION REPORT CHECKLIST
`
`D Re-initiation Authorized
`
`rn Confirmatory Testing Authorized D Other (List)
`SignatureJDate: __ -1~~-.._.,__.£~-'~"--___,. __ £_/_/.....,~-/_o....,y....__ ___ ___ _
`
`Action required
`
`Corrective Action
`
`b-U~'\cl -~ 5/1alo~
`
`Completed by
`
`Date
`
`M19.01
`Rev. 3
`
`•
`
`•
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Notebook 10750
`
`Page 021-\
`
`PRESERVATIVE RAW DATA
`
`•
`
`Product: AL-6221 0.004%0PH. SOLN.
`
`Lot number: 04-36405·2
`
`Sample Timepoint:
`On Test:
`04/21/2004
`
`Day 28
`
`Date of Sample:
`
`05/19/2004
`- - -- -- - -
`
`Organism Counts at Dilutions
`
`Plate Count
`Average
`
`Initials
`-Date
`
`Test Organism
`
`10·•
`
`S. aureus
`ATCC6538
`
`P. aeruginosa
`ATCC9027
`
`E. coli
`ATCC8739
`
`0
`0
`
`0
`
`0
`
`0
`
`0
`
`C. albicans
`ATCC 10231
`
`A. niger
`ATCC 16404
`
`•
`
`INTC
`
`\NTC
`
`\ /\lTl
`ll
`;>. 3
`
`\NT<...
`
`0
`
`\
`
`5
`)(. \ ()
`
`2.
`~.O'X\O
`
`MEDIA:
`
`Peptone Lot (tubes):
`
`N/A
`
`Saline Lot(tubes): Cl\-3bl.?~~-\ Polysallne Lot(tubes): Dl\-:,iotpl\\-\
`
`Peptone Lot (bulk):
`N/A
`Saline Lot (bulk):
`N/A
`Polysaline Lot (bulk):
`MCTA Lot: t.\ \ \ SL\ o le Waterbath Asset No.: ~J-;J. {Proo g ~\ Waterbath Temp(°C):
`Letheen Lot: Ot.\ -3Ll!u L\O - \
`_tJ_l'-A ________________ _
`Other:
`
`N/A
`
`ORGANISMS:
`
`A. nlger Preparation Reference: NIA
`---------
`
`Transfer Log Reference: N/A
`-----~
`
`M40.02
`Rev. 10
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`· - - -
`
`USP PRESERVATIVE EVALUATION SUMMARY
`
`Notebook 10750
`
`Page 021- 8
`
`••
`
`Product: AL-6221 0.004%0PH. SOLN.
`Preservative: NOf\lE ·UnpFe&erveJW~f;,,\cl-\ Date Assayed:
`Lot Number:
`04-36405-2
`Batch No.:
`Stability Data:
`
`FID No.:
`
`04/21/2004
`
`106039
`
`226270
`
`200193447
`
`Package:
`
`Procedure No.:
`
`Project No.:
`
`Initial
`---~-------
`150 m I
`PROC-0001136 (V-2.0)
`LIMS No.:
`SUMMARY OF RESULTS
`
`Or2anism Counts (CFU/mL or CFU/2)
`
`Test Organisms
`
`Initial
`
`7 Day
`
`14 Day
`
`28 Day
`
`S. aureus
`ATCC 6538
`
`P. a eruginosa
`ATCC9027
`
`E. coli
`ATCC8739
`
`C. albicans
`ATCC 10231
`
`A. niger
`ATCC 16404
`
`le ~ .-c x ,J
`\, D x \C>
`
`2.
`l . 1X \0
`
`L \O
`
`\ , \ "{.. \ 0
`
`lo
`
`3
`2.C\ )( 10
`
`\
`2.5x\O
`
`L\O
`
`~
`\, ~ x \o
`
`'\
`2 .:, x \0
`
`3
`<..1 x \ 0
`
`L.\0
`
`\. \ x \ 0
`
`~
`
`5
`1 ,5)( \0
`
`~
`<A .. C\ X \O
`
`s
`4. 3 x \o
`
`lg
`\ , \)(\ 0
`
`3
`\.OX\0
`
`.2.
`
`s.s )( \0
`
`~
`!2.. 0)l \ 0
`
`•
`
`Not Done (ND)
`
`Limits of Detection Established 0 _____ _ _ _ ____ _ _
`Limits of Detection Not Established ~
`
`.I "fhzlo~
`~ C.
`•..., '-"2 <i'{
`ail USP-&,W·JJ
`G""Pass USP Requirements
`t ~ ·1 JP
`JP R
`.
`.i:::.-~@.,...c -t-.J!-1_,.,./u-;l-~~--
`~p
`equ1remen s
`~ f ass
`a1
`/ ~--------·----
`~ .iJ . ., ii.l o<{
`\}ct.s.~ bd.~~ o("\ -two ..\.~c.h~; t.\c.n\s c:on \rm ct.lion~. C.
`. ~ ?-;).1011
`5 /i 1 ~---- ___ _
`Analyst: --~~Cl.)"\)'"LJ...
`e Verified By: ___ ~{~---- Date _ ;J?-z&}_/ __ _
`
`Date
`
`M40.03
`Rev. 6
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Page: 0 ;;l. / - C\
`Confirmation/Relnitiation Preservative Raw Data
`Formulation/Product: A l-- f.o ;)..d. I Oph . So/YI . P. F..
`- U 5 P-
`Lot Number: 04 ,3'4 Y.OS-;2.
`On Test: b-b.S' fol/-
`Date of Sample: see below
`Confirmation of: ~ • C..{) I i
`Reinitiation of: ~Al-=-+/~A~------
`Plate Count
`Average
`,.,
`/ .Ox 10
`
`Notebook: /07!%)
`
`105
`
`Initials
`-Date
`
`Sf ')8/al.j
`~
`~/4 /ov
`I:>.-
`~(It 0
`~
`;>-S fo'f
`
`t
`J . ~)(10
`... q ~
`!) . )(10
`
`~10
`
`- - - - - - .. -
`
`•
`
`Time point
`~
`.5/;)S' ol/
`~7
`<ol 1 Jo'f
`D~t'f
`u g/oc/-
`:D~ ;}.-~
`llh 1-/o
`
`I
`l e.
`
`Media/Organisms Used 16bsltN
`tp/F/oJI'
`'1/n/otf I'\
`"'I dot/
`()#. -;,t, 77/J,J ~ <l--3• 7'1?-/ ()¢-3/, 799-) ~ if,~'fff-J
`\.
`-
`Let.heeo
`-
`-
`-
`'\.
`Peptone Lot (tubes)
`f)c/--3{p 1hq-/ IJf-:7¥" 7111-1 !Otk~gOl -1
`\
`Polysaline Lot (tubes) Hit ,._, ..
`tJ/A
`Saline Lot (tubes)
`"''"' .
`-
`rJ/A-
`I !f.p.Gtlllof N/A
`£/ 11glfOfo L/l l~tf00 l/ If rt </ CXo 'ffL~J.07
`'
`A~545 A::;."'115'
`A-.:J~CK° A.;:1.595
`% .;;..
`-
`¥6.:J
`.!//,,. /
`Lf(., . lf
`-
`-
`-
`-
`-
`-
`-
`-
`-
`-
`-
`-
`1o31g: oc/~-').~
`
`v
`
`J
`
`JI I
`
`I
`
`{)<l-31(>5}4- 2
`
`MCTALot
`WaterbathAssetNo.
`Waterbath Temp. (oC)
`Pcptone Lot (bulk)
`Saline Lot (bulk)
`Poly511line Lot (bulk)
`A. niger Prep. Reference
`Transfer Log Reference
`Other:
`
`\
`\
`
`/
`7
`
`/
`
`/
`
`/
`
`-
`-
`-
`-
`-
`
`/
`
`/
`
`/
`
`I
`
`/
`
`/
`
`/
`
`\.
`
`/
`
`\
`/
`x
`\
`\
`'\
`\.
`f\..
`
`"'--
`
`..
`
`Analyst:
`
`'TY.;,/7,h•
`
`..-.
`filA ~-
`/ / / . . / Ll~ LJ
`Verified: ~~~b~ . h I tii-Cl .KJ"U..
`
`-/r 'V
`
`-
`
`<J
`
`Date: ~ /Bsio</
`u/f}..'5/ot.J
`
`Date:
`
`•
`
`M40.01
`Rev.3
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Notebook: ~/_t>~7_fl? ____ Page: o.:::!/ - \ 0
`
`I
`
`Confirmation/Reinitiation Preservative Raw Data
`Formulation/Product: ~AL.~--~-~-~' _fi~F _________________ _
`On Test: s.-p~/61/
`Lot Number: Ol( · ]II CfO)-- '2
`Date of Sample: see below
`Confirmation of: __.e .... -..... t"""'o"'""/._· ______ Reinitiation of: - - - - - - - - - -
`Plate Count
`Avera e
`
`Initials
`-Date
`
`7 Do.y
`"/1164
`It(/)<., y
`r, ft/aY
`7-8 l) ... y
`b IJ.i-/Gtf
`
`i, I
`0
`0
`
`(
`3
`
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`
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`
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`-
`
`0 'I· Jll 1'1'f-/ o 1..1-Jt.~01-1
`
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`
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`-
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`
`/
`
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`
`,
`
`/
`
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`
`I
`
`/
`
`/
`
`I
`
`I
`
`Media/Organisms Used 1 ... .-.J. • ..1 t..~I~ ~7 (),, 14 .
`::i_g
`IJLI..
`1>'1- ~i)/-1 :>'/-){, 11i- 1
`Letheen
`()L/· 'l,c,770 - 1 Im- Ji. ?'f'H
`-
`-
`Peptone Lot (tubes)
`-
`Saline Lot (tubes)
`-
`Polysaline Lot (tubes)
`ti I '3 'J'),o1
`MCI'ALot
`Ato:si
`Waterbath Asset No.
`Waterbath Temp. (-c)
`oAt, .O
`Peptone Lot (bulk)
`Saline Lot (bulk)
`Polysalinc Lot (bulk)
`A. niger Prep. lleference
`Transfer Log Reference
`Other:
`
`J031B :174& -z')...
`
`/
`Analyst: _.,.....;:.,~~....._...,....~· _,-- -- - - -- - --Date: _h'-'b'-t.-'-1<fll ___ _
`
`_,,Li=-><l...,n,...-b~J.rf\.4-~· '--=""=-->~=~-·-------- Date: _ IR_.;_/ 9.--'8~1 o_'=l....__ __
`
`I
`
`M40.0l
`Rev. 3
`
`Verified: _
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`USP PRESERVATIVE EVALUATION SUMMARY
`
`Notebook 10750
`
`Page 021-\\.
`
`•
`
`5/25/2004
`----------
`
`106039
`226270
`200193447
`
`Product: AL-6221 0.004% OPH. SOLN. PF CONFIRMATION OF E.coli
`-
`- --
`Date Assayed:
`
`Preservative:
`
`NONE
`
`Lot Number:
`
`Stability Data:
`
`Package:
`
`Procedure No.:
`
`04-36405-2
`
`Initial
`Bulk
`
`Batch No.:
`
`FID No.:
`
`Project No.:
`
`PROC-0001136, V-2.0
`SUMMARY OF RESULTS
`
`LIMS No.:
`
`Or anism Counts CFU/mL or CFU/
`
`Test Organisms
`
`Initial
`
`7 Day
`
`14 Day
`
`28Day
`
`•
`
`E. coli
`ATCC 8739
`
`/,fJx.1ofp
`
`,_,
`f.'J..x ro'f 5,~x ro
`
`~10
`
`C. a/bicans
`ATCC 1023 1
`
`Not Done (ND)
`
`Limits of Detection Established 0 ______ _ _
`Limits of Detection Not Established ~
`
`~ ~ss USP Requirements D Fail USP
`~Pass JP Requirements D Fail JP
`
`- - -- - - - - -
`
`Analyst: -4--1:-:£&'~~~~~~-~"----- Date: _b~-~-~/o__,__J( ___ _
`1/_~_..._f_o_,,7 ___ _
`_.:;.1,_
`
`Verified By:
`
`Date: _
`
`•
`
`M40.03
`Rev. 6
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`t {fV\f 'r~ ~ E r~.f'
`
`USP PRESERVATIVE EVALUATION SUMMARY
`
`Notebook 10750
`
`Page 021 - \ l
`
`•
`
`Product: AL6221 PF
`-------l~~~H~~~~~~~~M~>-t;~·~'---~~~~~~~~~-
`f VIV
`C7
`1 j yi./O l
`Preservative:
`ijNPRESERVED--
`Date Assayed:
`05/25/2004
`
`Lot Number:
`Stability Data:
`
`04-36405-2
`INITIAL
`
`Batch No.:
`FID No.:
`
`Package:
`150ML
`- - - - - - - -- - - - -
`Procedure No.:
`PRO C -0001136 v2.0
`LIMS No.:
`SUMMARY OF RESULTS
`Or anism Counts (CFU/mL or CFU/
`
`Project No.:
`
`106039
`
`226270
`
`200193447
`
`Test Organisms
`
`Initial
`
`7 Day
`
`14Day
`
`28Day
`
`•
`
`S. aureus
`ATCC6538
`
`P. aeruginosa
`ATCC9027
`
`E.coli
`ATCC8739
`
`C. albicans
`ATCC 10231
`
`A. niger
`ATCC 16404
`
`:>
`f. ( j( I 0
`
`Lt.. 0
`
`Not Done (ND)
`
`Limits of Detection Established 0 ______________ _
`t§/
`Limits of Detection Not Established
`
`B Pass USP Requirements D Fail USP
`Gr Pass JP Requirements D Fail JP - - - - - - - -
`
`Analyst: ___.~~~-~-' _
`
`•
`
`Verified By: _
`
`_
`
`M40.03
`Rev. 6
`
`_~---- Date: _t,__,_fM~/q __
`'1-/ vy'o 9
`
`Date:
`
`I
`
`1
`f-- _
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`AIPelResults.05.LIMS126.0.072004
`
`Database: LIMSAR
`
`!l-.>
`0
`0
`<.ft
`..1
`0
`
`I --
`
`Report Approved by: Ronald Berry on 27..JUL-200410:08am
`
`Limits of Detection: Not Established
`
`Passes USP & JP
`
`2.0E2
`4.3E5
`<10
`<10
`<10
`
`8.5E2
`8.9E5
`6.7E3
`2.5E1
`2.2E2
`
`1.0E3
`7.5E5
`2.3E4
`2.9E3
`8.0E3
`
`1.1E6
`1.1 E6
`1.2E6
`1.1 E6
`1.0E6
`
`28DAY
`
`14 DAY
`
`7DAY
`
`INIT
`
`Comments:
`Result Summary:
`
`USP: PASS
`JP: PASS
`
`ATCC16404
`ATCC10231
`ATCC8739
`ATCC9027
`ATCC6S38
`
`Test Organism
`
`300922630 ,300922631
`
`10750:021
`
`Ref#:
`Project No.: 226270
`Preservative: NONE
`Task IDs:
`
`Package: Corning Filter Unit/ 150 ml
`Stability Data Initials
`Product: AL6221 0.004% OPH. SOLN. (PRESERV
`Submission ID: 100074746
`
`Method:
`Date Assayed: 21-APR-2004
`Series No.:
`User Sample ID: Batch NO 04-36405-2,LN 9988:087
`Sample ID:
`
`200193447
`
`PET, USP
`
`106039
`
`Page 1 of 1
`
`• USP Preservative Evaluation 6mary
`
`(MTP PROC-0001136 (V-2.0))
`
`Report Date: 12-AUG-2004 03:19 PM
`
`• Alcari
`
`R&DLIMS
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Alcari
`R&DLIMS
`
`•
`
`LIMS Submission ID: 100074746
`ReQuester
`: Kabra Bhagwati
`Customer Datagroup
`: FO RMULATION OEVELOPMEN
`Logged By
`: SRUGWANI
`
`Project Number
`226270
`Mail Code
`R3-53
`Telephone Extension : 8193
`CC : Reports To
`SRUGWANI
`
`\ 0\50: O'C}. l - \<{
`Intermediate Sample Results Report
`Report Date: 12-AUG-2004 03:18 PM
`
`Page 1of 1
`
`Sample Information
`
`LIMS Sample ID
`Sample Description
`Sample Type
`Material Name
`Materi al Type
`LaboratoryfSupv.
`Specific Location
`Date Logged
`
`=200193447
`: Batch NO 04-36405-2,LN 9988:087
`: 106039 AL6221 0.004'/o OPH. SOLN. (PRESERV
`:SOLUTION
`:A NEW MATERIAL TYPE
`: MICROBIOLOGY
`: PET LAB
`: 04/15/2004
`
`•
`
`AGE
`DATE NEEDED
`FORMULATION ID
`LABORATORY
`NUMBER OF UNITS
`PKG/FILL VOL
`PURPOSE
`STORAGE CONDITION
`
`: Initials
`: 04-29-04
`: 106039
`: MICROBIOLOGY
`: 1
`: Corning Filter Unit / 150 ml
`: MICROBIOLOGY STUDY
`: RT.AMBIENT
`
`Result Information
`Task ID
`Component
`300922630 USP
`300922630
`JP
`300922630 RESULT SUMMARY
`300922630
`LIMITS OF DETECTION
`
`Task Information
`
`Task ID
`
`Method
`
`300922630 PET, USP
`
`REFERENCE NUMBER
`WORK DONE BY
`PROCEDURE NUMBER
`DATE RECEIVED
`DATE ON TEST
`PRESERVATIVE
`
`10750'021
`GUTIERREZC
`. PROC..()()01136 (V-2 0)
`16·APR-04
`. 21-APR-04
`NONE
`
`Result Value
`PASS
`PASS
`Passes USP & JP
`Not Established
`
`Units
`
`Rep
`
`Procedure
`
`PET, USP
`
`Method
`Datagroup
`
`Condition
`
`MICRO-ALL
`
`APPROVED
`
`Report Approved by: Ronald Berry on 27..JUL-2004 10:08am
`
`•
`
`Database: UMSAR
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`AISampleResults.07.UMS110.1.012004.P0002241
`
`
`
`Ale<11i
`R&DLIMS
`
`•
`
`LIMS Submission ID : 100074746
`: Kabra Bhagwati
`Requester
`Customer Datagroup
`: FORM ULATION D EVELOPMEN
`Logged By
`: SRUGWANI
`
`Project Number
`226270
`Mail Code
`R3-53
`Telephone Extension : 8193
`CC : Reports To
`SRUGWANI
`
`lO"l ~o·. Cd.. \ - \ C:::,
`Intermediate Micro Sample Results Report
`Report Date: 12-AUG-2004 03:21 PM
`
`Page 1 of2
`
`Sample Information
`
`LIMS Sample ID
`Sample Description
`Sample Type
`Material Name
`Material Type
`l aboratory/Su pv.
`Specific Location
`Date Logged
`
`:200193447
`: Batch NO 04-36405-2,LN 9988:087
`: 106039 AL6221 0.004% OPH. SOLN. (PRESERV
`: SOLUTION
`:A NEW MATERIAL TYPE
`: MICROBIOLOGY
`: PET LAB
`: 04/15/2004
`
`AGE
`DATE NEEDED
`FORMULATION ID
`LABORATORY
`NUMBER OF UNITS
`PKG/FILL VOL
`PURPOSE
`STORAGE CONDITION
`
`: Initials
`: 04-29-04
`: 106039
`: MICROBIOLOGY
`: 1
`: Coming Filler Unit / 150 ml
`: MICROBIOLOGY STUDY
`: RT.AMBIENT
`
`Units
`
`Rep
`1
`
`1
`
`1
`
`1
`1
`
`1
`1
`
`Result Value
`PASS
`PASS
`Passes USP & JP
`Not Established
`1.0E6
`1.1E6
`1.2E6
`1.1E6
`1.1E6
`8.0E3
`2.9E3
`2.3E4
`7.SES
`1.0E3
`2.2E2
`2.5E1
`6.7E3
`8.9E5
`8.5E2
`<10
`<10
`<10
`4.3E5
`2.0E2
`
`AISampleResults.07.LIMS 110.1.012004.P0002241
`
`•
`
`Result Information
`Task ID
`Com~onent
`300922630 USP
`JP
`300922630
`300922630 RESULT SUMMARY
`LI MITS OF DETECTION
`300922630
`300922631 ATCC6538 -INIT
`300922631 ATCC9027 -INIT
`300922631 ATCC8739 -I NIT
`300922631 ATCC10231-INIT
`300922631 ATCC16404-INIT
`300922631 ATCC6538 -7 DAY
`300922631 ATCC9027 -7 DAY
`300922631 ATCC8739 -7 DAY
`300922631 ATCC10231 -7 DAY
`300922631 ATCC16404-7 DAY
`300922631 ATCC6538 -1 4 DAY
`300922631 ATCC9027 -14 DAY
`300922631 ATCC8739 -1 4 DAY
`300922631 ATCC10231-14 DAY
`300922631 ATCC16404-14 DAY
`300922631 ATCC6538 -28 DAY
`300922631 ATCC9027 -28 DAY
`300922631 ATCC8739 -28 DAY
`300922631 ATCC10231 -28 DAY
`300922631 ATCC16404-28 DAY
`
`•
`
`Database: U MSAR
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`
`
`Alcari
`R&D LIMS
`
`•
`
`l01'So : o~ \- l~
`Intermediate Micro Sample Results Report
`Report Date: 12-AUG-2004 03 :21 PM
`
`Page 2 of 2
`
`LIMS Submission ID : 10007 47 46
`Requester
`: Kabra Bhagwati
`Customer Datagroup
`: FORMULATION OEVELOPMEN
`Logged By
`: SRUGWANI
`
`Project Number
`226270
`Mail Code
`R3-53
`Telephone Extension : 8193
`CC: Reports To
`SRUGWANI
`
`Sample Information
`:200193447
`: Batch NO 04-36405-2,LN 9988:087
`:106039 AL6221 0.004% OPH. SOLN. (PRESERV
`:SOLUTION
`:A NEW MATERIAL TYPE
`: MICROBIOLOGY
`:PET LAB
`: 04/15/2004
`
`LIMS Sample ID
`Sample Description
`Sample Type
`Material Name
`Material Type
`laboratory/Supv.
`Specific Location
`Date Logged
`
`Result Information
`Task ID
`Component
`
`Result Value
`
`Units
`
`Rep
`
`Confirmation for E.coli
`
`Initial
`Day 7
`Day 14
`Day 28
`
`Tech 1 Tech 2
`1. 0EB
`1.3E6
`1.2E4
`1.9E4
`5.9E2
`1. 1E3
`<:10
`<:10
`
`Task Information
`
`•
`
`Task ID
`
`Method
`
`300922630 PET, USP
`
`REFERENCE NUMBER
`WORK DONE B Y
`PROCEDURE NUMBER
`DATE RECEIVED
`DATE ON TEST
`PRESERVATIVE
`
`. 10750:021
`. GUTIERREZC
`. PROC-0001136 (V-2 0)
`. 16-APR--04
`21-APR--04
`. NONE
`
`Procedure
`
`Method
`Oatagroup
`
`Condition
`
`PET, USP
`
`MICRO-ALL
`
`APPROVED
`
`300922631 PET, USP SUMMARY
`
`PET, USP SUMMARY
`
`MICRO-ONLY APPROVED
`
`Report Approved by: Ronald Berry on 27-JUL-2004 10:08am
`
`•
`
`Database: LIMSAR
`
`CONFIDENTIAL – PROTECTIVE ORDER MATIERAL
`
`AISampleResulls.07 .LIMS110.1.012004P0002241
`
`
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