{ ,,
`\
`
`I
`‘
`
`_,»
`
`A Division of Albany Molecular Research Inc.
`
`,_
`
`Kent Avenue
`es Lafayette, IN 47906-1076
`Phone (765)46.
`2
`Fax (765)463-4
`sscl-Inc com
`E-maul
`|nfo@
`web www sscmnc com
`
`Chromatographic Data from
`the Stability Evaluation of
`Bromfenac Sodium Drug
`Product Samples for Potency
`
`Project ID: EL20l5l326
`Report Date:
`I/I2/2016
`
`CONFIDENTIAL
`
`PAGE 1 OF 53
`
`PROL0337648
`SENJU EXHIBIT 2266
`
`LUPIN v SENJU
`
`IPR2015—01 100
`
`

`
`I.
`
`SUMMARY
`
`This document contains chromatographic stability da ta from the analysis of Bromfcnac sodium
`ophthalmic solution drug product for potency. Samples were sourced from Scnju.
`
`Table I. Summary of HPLC Data. Sequence 74l88I
`
`Sample
`
`,
`
`
`
`1m—j11 5
`E5188 6
`7
`11
`741885
`12
`741886
`13
`741887
`14
`741888
`15
`741889
`741890 ‘— 16
`741897
`17
`741898
`18
`741899
`19
`741900
`20
`741901
`21
`
`so A
`sm A
`STD A
`570 A
`sro B
`
`STD A
`240031
`240031
`240031
`sro A
`
`408705
`408705
`408705
`408705
`408706
`408677
`408705
`403486
`403489
`403490
`408705
`
`Clirvtnulogrupltir Data from the Stability I-Ivaluation ofBromfcnac Sodimn Drug Product Santplcs for Potemjr, l/I2/20I6,
`page 2 of 53
`
`CONFIDENTIAL
`
`PAGE 2 OF 53
`
`PROL0337649
`
`

`
`Table 2. Summary of HPLC Data. Sequence
`
`s°"'p'°
`Description
`
`STD A
`STD A
`STD A
`STD A
`STD A
`STD B
`
`STD A
`STD A
`STD A
`STD A
`STD A
`STD A
`STD A
`STD A
`240031
`240031
`240031
`240031
`240031
`240031
`STD A
`240031
`
`240031
`240031
`STD A
`
`LIMS LC F ename
`408577
`742200
`408677
`742201
`408705
`742202
`408705
`742203
`408705
`742204
`408705
`742205
`403705
`742206
`408706
`742207
`408677
`742208
`408705
`742215
`408705
`742222
`408705
`742229
`408705
`742235
`408705
`742242
`408705
`742249
`408705
`742256
`408705
`742262
`403478
`742263
`403479
`742264
`403480
`742265
`403481
`742266
`403482
`742267
`403483
`742268
`408705
`742269
`403484
`742272
`403485
`742273
`403487
`742274
`403488
`742275
`408705
`742276
`
`RT
`
`Area(mAU's)
`
`Page
`
`8.669
`8.670
`8.670
`8.670
`8.669
`8.669
`
`8.673
`8.676
`8.677
`8.681
`8.682
`8.684
`8.690
`8.691
`8.670
`8.670
`8.670
`8.673
`8.671
`8.672
`8.694
`8.676
`8.676
`8.678
`8.680
`8.701
`
`4011.82
`
`4010.89
`4010.87
`
`4055.66
`
`4015.87
`4019.08
`4018.56
`4017.59
`4019.84
`4017.62
`4017.27
`4023.48
`4537.86
`4545.41
`4541.65
`4522.94
`4555.21
`
`4024.68
`4541.95
`4541.17
`4524.65
`4523.19
`4024.02
`
`OJ 0-
`
`\l
`
`B 0-4
`
`J5\l
`
`D-‘
`N
`
`('I1rvImII0m‘aphIk.'l)aIu fl'am the Stability Ifrnlualion ofBromfvnac Sodimn Drug Product Sarnplcs for Polemjv, l/I2/20I(»,
`page 3 of 53
`
`CONFIDENTIAL
`
`PAGE 3 OF 53
`
`PROL0337650
`
`

`
`ll. CHROMATOGRAMS
`
`( 'I:romumgruplrir I )uIa ji'om the Sluhi/iI_r Ifraluulion Q/‘Iirmn/iwuc Sodium I)rug I’rodu(I SmnpIv.\- for I’oIomjr, I“ I 2I2()|(u,
`pugc 4 of 53
`
`CONFIDENTIAL
`
`PAGE 4 OF 53
`
`PROLO337651
`
`

`
`Data File D:\l.IHSOATA\741882.D
`nllannnnnncnlllnllullItIInIIuIIxx:nu:I21::nu:llnunlnuunnsxnnunxnnnlln
`Iniection Date
`11/16/2015 5:01:26 Pl!
`Sea. Line :
`1
`Supple Hue
`408677
`Locecion : V1.91 1
`Ace. Oneracor
`GT
`In1 :
`1
`Aca. Insuulent
`Inscrunenc 1
`In) Volune : S 111
`Sequence hie
`D: \ LIHSDATA\74188l . S
`lechod
`C: \HPCHEH\ l\HITHODS\62940t502 .H
`.
`.
`.
`
`.uuuuuu
`
`DAD1 A. Sag-206.4 ea-3oo.1oo'c741se2.o)
`
`Suple Nunez 408677
`
`150
`
`1%
`
`:s:::::::::::=::u::n::::=:332:x:3::=:uan=:ax::::n:::::u::::::::n::x::
`Area PQKCCYIC RCDOIXC
`nun-nun-:-----an-n----u--Inunn-nansnnnn-unsun---nun:-3--I--a--n--an-I
`
`sicmal
`:
`sorted Bv
`11/16/2015 2:21:49 PH
`Calib. Data loditxed :
`1.0000
`luluoliez
`:
`1 . 0000
`Diluczon
`'
`Use Hulupliez 5. Dilution Factor Inth ISTD:
`
`Signal 1: DAN. A, 519-266,‘! Re!-360,100
`Nae
`Area
`Peak RetTiIe ‘Noe
`lhdth
`Area
`=1:
`I
`[min]
`r um f|AU*:1
`—--—l ----- --I ---- --4 ----- --I -------- -—| ------- -—a ------------------- --
`1
`8.100
`0.0000
`0.00000
`0.0000 Bzontenec
`
`Totals :
`
`0.00000
`
`Results obtained with enhanced integrator‘
`1 Uazninq: or Errors :
`
`llezninq : Canbrated conpound(:) not round
`nn--nun-:annInn:-nnunInnInunnannnnxx:nnnu:nu:nnnunnnnxnnxnnxxxxn-nun:
`*" End 02 Report "*
`
`Insczunenr. 1 11/16/2015 5:14:25 PH GT
`
`Page 1 0t 1
`
`( Vpronmlographic Dalafrom the Stability I-.'ra/nation nfBrong/lmnc Sodium Drug Producl Samples _/hr l’oIwx'_\'. I/I2/20l6,
`page 5 of 53
`
`CONFIDENTIAL
`
`PAGE 5 OF 53
`
`PROL0337652
`
`

`
`Data File D:\l.IHSOATA\741883.D
`nllannnnnnunslllllullItIInIIIIIIn::1II21::nu:slnunlnuln-Ixnnunlsnnlln
`Iniection Date
`11/16/2015 5:16:11 Pl!
`Sea. Line :
`2
`Supple Hue
`408677
`Locecion : V1.91 1
`Ace. Oneracor
`GT
`In1 :
`1
`Aca. Insuulent
`Inscrunenc 1
`In) Volune : S 111
`Sequence hie
`D: \ LIHSDATA\74188l . S
`lechod
`C: \HPCHEH\ l\HITHODS\62940t502 .H
`.
`.
`.
`
`.uuuuuu
`
`DAD1 A. s..-2oo.4 ea-3oo.1oo'(741es3.o)
`
`Suple Nunez 408677
`
`150
`
`1%
`
`:s:::::::::::=::u::n::::=:332:x:3::=:uan=:ax::::n:::::u::::::::n::x::
`Area PQKCCYIC RCDOIXC
`nun-nun-:-----an-n----u--Inunn-nansnnnn-unsun---nun:-3--I--a--n--an-I
`
`sicmal
`:
`sorted Bv
`11/16/2015 2:21:49 PH
`Calib. Data loditxed :
`1.0000
`luluoliez
`:
`1 . 0000
`Diluczon
`'
`Use Hulupliez 5. Dilution Factor Inth ISTD:
`
`Signal 1: DAN. A, 519-266,‘! Re!-360,100
`Nae
`Area
`Peak RetTiIe ‘Noe
`lhdth
`Area
`=1:
`I
`[min]
`r um f|AU*:1
`—--—l ----- --I ---- --4 ----- --I -------- -—| ------- -—a ------------------- --
`1
`8.100
`0.0000
`0.00000
`0.0000 Bzontenec
`
`Totals :
`
`0.00000
`
`Results obtained with enhanced integrator‘
`1 Uazninq: or Errors :
`
`llezninq : Canbrated conpound(:) not round
`nn--nun-:annInn:-nnunInnInunnannnnxx:nnnu:nu:nnnunnnnxnnxnnxxxxn-nun:
`*" End 02 Report "*
`
`Insczunent 1 11/16/2015 5:29:10 PH 61‘
`
`P190 1 91 1.
`
`( Vpronmlographic Dalafrom the Stability I-.'ra/nation nfBrong/lmnc Sodium Drug Producl Samples _/hr l’oIwx'_\'. I/I2/20l6,
`page 6 of 53
`
`CONFIDENTIAL
`
`PAGE 6 OF 53
`
`PROL0337653
`
`

`
`Data File D:\LIH$DATA\'Ml8Bd.D
`
`
`
`
`Sanple liane: 408705
`
`
`
`
`
`Extended
`
`Instrument:
`Instrument 1
`
`
`
`
`
`rertornsnce Report
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`nodule
`Firmware revision Serial number
`
`
`
`
`
`__________________________________ __I___-_.-____________|_____-_________
`1100 Ouaternerv Puma
`.I..05..I.1 F0131
`11370201400
`
`
`
`
`
`
`
`1100 Autoselfller
`.\.D5..Ll
`|'D13'|
`US'?|32D1352
`
`
`
`
`
`
`1.100 Diode Arrev Detector
`1.05.11 F0131
`l.FS6ddl3|3691
`
`
`
`
`
`
`
`DE63B6415B
`11.00 Coluln Therlostat
`5.05.11 [013]
`
`
`
`
`
`
`
`Software Revision: RGO’. 1.10.02 [1757] Compriqht G Afiilent Technologies
`
`
`
`
`
`
`
`
`
`
`
`
`Coluan Destrintion : Shiseido Cancel]. Pal: C18
`
`
`
`
`
`
`Product!
`Baitchl‘:
`:
`12503
`
`Serial!
`: M013 M232
`
`
`2.1 II
`Diameter
`:
`
`5.0 no
`Particle size
`:
`
`
`
`
`400 bar
`Haximun Pressure
`:
`
`
`
`
`
`0 ‘C
`Haxiuun Tennerature:
`
`
`
`
`Content
`: LIBS 405201
`
`
`
`
`
`100.0 II
`
`68.0 %
`11
`
`
`
`
`
`Lennrth :
`
`Void volume :
`
`
`llaxinun pl-I
`:
`
`
`
`
`
`
`
`
`
`
`
`l3:\I'IPCI'llZll\1\HE1'li0'DS\62l94fl5D1.K
`Analysis nethod:
`
`
`
`
`
`Samnle intonation tor Location:
`
`
`
`Saunle Ilene:
`400105
`
`
`
`Iniectionl:
`J.
`
`
`5 ul
`Injection volune:
`
`
`
`Acquisition intonation:
`
`
`
`
`
`1.00
`1.00
`
`
`
`
`
`Eultiolier:
`Dilution:
`
`
`
`
`
`Via]. 2
`
`
`
`
`
`
`Uoerator:
`GT
`
`
`11.-"16.r'2D15 5:31:14 Pl!
`Dateffile:
`
`
`
`
`D:\LI!l5Dfi.T.l\'}41064.D
`Date tile nale:
`
`
`
`
`Itethod tile nane: C:\I-IPCI-I!.'H\1\H£‘1'I-I01)$\62:940501.!*l
`
`
`
`
`
`
`
`1.500
`nlfnin
`flow:
`
`
`
`
`115 bar
`Pressure at start:
`
`
`
`
`2S.J.‘C
`Lett Tenn. at start:
`
`
`
`
`Right Tenp. at start: 25.0'l3
`
`
`
`
`Solvents:
`
`Pressure at end:
`
`
`
`Luett Team. at end:
`
`
`
`
`Right ‘Tenp. at end:
`
`
`
`
`FHPI. Solvent A6294-05-01 {exp 1Z!l6)'15)
`
`
`
`
`
`
`PHP1. Solvent 3
`
`
`
`PHI-'1. Solvent 12
`
`
`
`MP1, Solvent D
`
`
`
`
`
`
`
`
`117 box,
`
`‘C
`25.:
`
`
`25.0 ‘C
`
`
`
`
`
`
`
`Signal description: DAD1 L, Sic-v266,4 Re:-660,100
`
`
`
`
`
`
`
`
`Instrument 1 1.'|J16!2E|15 5:44:14 PH 61'
`
`
`
`
`
`
`
`Page J. oi «I
`
`Chrorraatagruphfc Datafrom the Srabihry Emfuarion ofBr'omfem:c Sodfrrm Drug Product Sampfearfor Potency, l!12!20 16,
`
`
`
`
`
`
`
`
`
`
`
`
`
`page 7 of 53
`
`
`
`
`
`
`CONFIDENTIAL
`
`
`
`PAGE 7 OF 53
`
`PROL0337654
`
`
`
`PAGE 7 OF 53
`
`

`
`Dace rue D:\LnlSDA1'A\74188-1.0
`DAD1 A. Sif2@.4 RQVIWAM (M18910)
`
`Suple Ilene: 408705
`
`
`
`Insuunent 1 11/16/2015 5:44:14 PH 61'
`
`up 2 ol 4
`
`Chrmnulographic Datafrom the Stability I'.'mIuaIi0n nfflrnmfenac Sodium Dmg I’roducI Salnples jbr Polencjr, I/I2/20I 6,
`page 8 of 53
`
`CONFIDENTIAL
`
`PAGE 8 OF 53
`
`PROL0337655
`
`

`
`Date Fl 1: D: \ LIIISDATM741884. D
`
`: Bzontenac
`Conoundl 1
`Anounr.( nq/nu): 0.0000
`
`Sample line: 408705
`
`Peak description mm:
`Sumol: DAD1 A, 51¢-266.4 Re!-360.100
`Refine: 8.667
`k‘:
`54. 199
`4012.7
`Hnuhc:
`228.15
`Area:
`Scan:
`8.365
`End:
`9. 952
`Skeu:
`0.888
`Excess:
`. 577
`. 270
`llxdch at nu: hemht:
`. $8‘!
`5 none:
`unaenc:
`. 478
`. S73
`t.a111nq:
`. 454
`svueuv:
`. 771
`USP Tuhna:
`33
`Inceazauon tvbe:
`‘hue xnczcnnc (Inc):
`Data pomcs:
`
`D-00000!-
`
`
`
`Suuaucol nonents (83 peak detecuon):
`H0:
`4011.8
`H1:
`8.738
`Tanaent method
`H2:
`0.016448
`floltlndch nethod
`H3:
`0. 001874
`5 sun; uechod
`H4:
`0.001238
`Scetlsucol
`
`Etncxcncvz Plates nu:
`COIUII1
`S251
`S709
`S457
`4642
`
`..
`I258!
`S2510
`S7088
`54566
`46423
`
`Relauonshm to preceedma beak:
`Resoluuon Tanaenr. Iechod:
`Ihltuxdth method
`
`Selecuvxtv:
`5 Man method
`Steustical nethod
`
`Instrument 1 11/16/2015 5:44:14 P)! G!‘
`
`One 2 ol 4
`
`(Wromalographic Datafrom Ihe Slabiliry l'.'\'aIuaIion ofBromfvnac Sodium Dnlg I’rodu¢'I Samples for Polencjr, II I 2/20|6.
`page 9 of 53
`
`CONFIDENTIAL
`
`PAGE 9 OF 53
`
`PROL0337656
`
`

`
`Data rue D:\l.IlIsDATA\741884.D
`I Ret.Tne
`Anount
`lnml
`Ina/ull
`
`1“‘ 3.667‘
`Total:
`
`0.0000"
`0.0000
`
`lane
`
`Pace
`I
`
`a:on:enac"
`
`3
`
`-'- End 0! Report -'1
`
`Se-pie Ilene: 408705
`
`Inscrunenr. 1 11/16/2015 5:44:14 PH GT
`
`up 0 ol 1
`
`( 'hr0muIograpIu'c I)aIafrom the Slnhilily I'.'\'nIuaIion Q/‘Iirom/i'nac Sodium Drug I’roducI Samples jbr I’vIenc_r. I.’ I 2/20l 6,
`page I0oI‘53
`
`CONFIDENTIAL
`
`PAGE 10 OF 53
`
`PROL0337657
`
`

`
`Data File D:\LIHsDATA\74188S.D
`STD A
`
`Senple Name: 408705
`
`: 11/16/2015 5:46:26 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-266.4 Re!-150.100 (7418851))
`
`MAU
`
`4
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : 5 ul
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hulupner c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ __ __' _ _ _ _ — __| _ _ _ . _ _ _ _ __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.668 88
`0.2694 401S.13452 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`0015. 13452
`
`Results nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 5:59:25 PH GT
`
`Page lot 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/20l6,
`pagell of53
`
`CONFIDENTIAL
`
`PAGE 11 OF 53
`
`PROL0337658
`
`

`
`Data File D:\LIHsDATA\741886.D
`STD A
`
`Senple Name: 408705
`
`: 11/16/2015 6:01:13 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-266.4 Re!-150.100 (7418861))
`
`MAU
`
`5
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : S n1
`
`
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`C0111). Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ — __| _ _ _ _ _ _ _ _ __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.666 PP
`0.2674 4016.96460 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`001636460
`
`Result: nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid ca11brat1on curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 6:14:11 PH GT
`
`:19. lot 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/20l6,
`pagel2of53
`
`CONFIDENTIAL
`
`PAGE 12 OF 53
`
`PROL0337659
`
`

`
`Data File D:\LIHsDATA\741887.D
`STD A
`
`Senple Name: 408705
`
`: 11/16/2015 6:15:57 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-206.4 Re!-ZbO.1OO (7418870)
`
`MAU
`
`6
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : 5 ul
`
`
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hulupner c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ __ __' _ _ _ _ — __| _ _ _ _ _ _ _ _ __I _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.666 88
`0.2675 4016.03931 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`G016.0393l
`
`Result: nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 6:28:55 PH GT
`
`:19. lot 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/20l6,
`pagel3of53
`
`CONFIDENTIAL
`
`PAGE 13 OF 53
`
`PROL0337660
`
`

`
`Data File D:\LIHsDATA\741888.D
`STD A
`
`Senple Name: 408705
`
`: 11/16/2015 6:30:41 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence Fue
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-206.4 Re!-ZbO.100 (7418880)
`
`MAU
`
`7
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : S n1
`
`
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`C0111). Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ — __| _ _ _ _ _ _ _ _ __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.666 B?
`0.2695 4018.79224 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`0018319224
`
`Result: nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 6:43:40 PH GT
`
`:19. 1°: 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/20l6,
`pagel4of53
`
`CONFIDENTIAL
`
`PAGE 14 OF 53
`
`PROL0337661
`
`

`
`Data File D:\LIHsDATA\741889.D
`STD B
`
`Senple Name: 408706
`
`: 11/16/2015 6:45:24 PH
`Imection Date
`: 403706
`sannle Rene
`: GT
`Ace. Operator
`Acct. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-266.4 Re!-150.100 (7418890)
`
`MAU
`
`8
`Sea. Line :
`Locet1on : V101 3
`In1 :
`1
`Inj Volune : 5 1:1
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renorvt
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`Sitmol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hulupner c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1. A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ __ __' _ _ _ _ _ __| _ _ _ _ _ _ _ _ __. _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8. 665 PB
`0. 2677 4038. 44849 100. 0000 Brontenec
`
`Nam.-
`
`Totals :
`
`0038. 44849
`
`Results nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 6:58:24 PH 01'
`
`Page 1 cl 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/2016,
`pagel5of53
`
`CONFIDENTIAL
`
`PAGE 15 OF 53
`
`PROL0337662
`
`

`
`Data File D:\l.IHSDATA\741890.D
`nllannnnnncnlllnnlullItIInIIIanIn::1II21::nu:llnunlnulnnsxnnunnnnnlln
`Iniection Date
`11/16/2015 7:00:09 Pl!
`Sea. Line :
`9
`Supple Hue
`408677
`Locecion : V1.91 1
`Ace. Oneracor
`GT
`In1 :
`1
`Aca. Insuulent
`Inscrunenc 1
`In) Volune : S 111
`Sequence hie
`D: \ LIHSDATA\74188l . S
`lechod
`C: \HPCHEH\ l\HITHODS\62940t502 .H
`.
`.
`.
`
`.uuuuuu
`
`DAD1 A. Sag-206.4 ea-3oo.1oo'c741e9o.o)
`
`Suple Nunez 408677
`
`150
`
`1%
`
`:s:::::::::::=::u::n::::=:332:x:3::=:uan=:ax::::n:::::u::::::::n::x::
`Area PQKCCYIC RCDOIXC
`nun-nun-:-----an-n----u--Inunn-nansnnnn-unsun---nun:-3--I--a--n--an-I
`
`sicmal
`:
`sorted Bv
`11/16/2015 2:21:49 PH
`Calib. Data loditxed :
`1.0000
`luluoliez
`:
`1 . 0000
`Diluczon
`'
`Use Hulupliez 5. Dilution Factor Inth ISTD:
`
`Signal 1: DAN. A, 519-266,‘! Re!-360,100
`Nae
`Area
`Peak RetTiIe ‘Noe
`lhdth
`Area
`=1:
`I
`[min]
`r um f|AU*:1
`—--—l ----- --I ---- --4 ----- --I -------- -—| ------- -—a ------------------- --
`1
`8.100
`0.0000
`0.00000
`0.0000 Bzontenec
`
`Totals :
`
`0.00000
`
`Results obtained with enhanced integrator‘
`1 Uazninq: or Errors :
`
`llezninq : Canbrated conpound(:) not round
`nn--nun-:annInn:-nnunInnInunnannnnxx:nnnu:nu:nnnunnnnxnnxnnxxxxn-nun:
`*" End 02 Report "*
`
`Insczunent 1 11/16/2015 7:13:07 PH 01‘
`
`P190 1 91 1.
`
`( Vpronmlographic Dalafrom the Stability I-.'ra/nation nfBrong/lmnc Sodium Drug Producl Samples _/hr l’oIwx'_\'. I/I2/20l6.
`page l6ol'53
`
`CONFIDENTIAL
`
`PAGE 16 OF 53
`
`PROL0337663
`
`

`
`Data File D:\LIHsDATA\741897.D
`STD A
`
`Senple Name: 408705
`
`: 11/16/2015 3:43:13 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-206.4 Re!-ZbO.1OO (7418970)
`
`MAU
`
`16
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : S n1
`
`
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 P11
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ _ __| _ _ _ _ _ _ _ _ __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.666 PP
`0.2677 4019.73315 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`0019313315
`
`Result: nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 8:56:11 PH GT
`
`:19. lot 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/2016,
`pagel7of53
`
`CONFIDENTIAL
`
`PAGE 17 OF 53
`
`PROL0337664
`
`

`
`Data File D:\LIHsDATA\741898.D
`240031
`
`Senple Kane: 403486
`
`: 11/16/2015 3:57:59 PH
`In1ect1on Date
`: 403486
`sample Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`c:xupcutnx1\nm1nons\s294oso2.n
`.
`.
`,
`DAD1 A. Sig-266.4 Re!-150.100 (7418980)
`
`MAU
`
`17
`Sea. Line :
`Locet1on : V101 10
`In1 :
`1
`Inj Volune : S n1
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 P11
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rI1U*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ — __| _ _ _ _ _ _ _ _ __. _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.646 B?
`0.2741 4556.1$869 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`4556. 15369
`
`Results nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 9:10:57 PH GT
`
`:19. 101 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/2016,
`pagel8of53
`
`CONFIDENTIAL
`
`PAGE 18 OF 53
`
`PROL0337665
`
`

`
`Data File D:\LIHsDATA\741899.D
`240031
`
`Senple Kane: 403489
`
`: 11/16/2015 9:12:44 PH
`Imection Date
`: 403489
`sample Rene
`: GT
`Ace. Operator
`Acct. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-266.4 Re!-150.100 (7418990)
`
`MAU
`
`18
`Sea. Line :
`Locet1on : V101 11
`In1 :
`1
`Inj Volune : S 1:1
`
`800
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renorvt
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`Sitmol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`C0111). Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD]. A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ _ __| _ _ _ _ _ _ _ — __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8. 648 PP
`0. 2721 4548. 27100 100. 0000 Brontenec
`
`Nam.-
`
`Totals :
`
`0548. 27100
`
`Results nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 9:25:41 PH 01'
`
`Page 1 cl 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/2016,
`pagel9of53
`
`CONFIDENTIAL
`
`PAGE 19 OF 53
`
`PROL0337666
`
`

`
`Data File D:\LIHsDATA\741900.D
`240031
`
`Senple Kane: 403490
`
`: 11/16/2015 9:27:27 PH
`Imection Date
`: 403490
`sannle Rene
`: GT
`Ace. Operator
`Acct. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`c:xupcutnx1\nm1nons\s294oso2.n
`.
`.
`,
`DAD1 A. Sig-266.4 Re!-150.100 (7419000)
`
`MAU
`
`19
`Sea. Line :
`Locet1on : V101 12
`In1 :
`1
`Inj Volune : S 111
`
`800
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renorvt
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`Sitmol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`C0111). Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ _ __| _ _ _ _ _ _ _ _ __. _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8. 647 PP
`0. 2721 4547. 03369 100. 0000 Brontenec
`
`Nam.-
`
`Totals :
`
`4547. 03369
`
`Results nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 9:40:24 PH 01'
`
`Page 1 cl 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/2016,
`page20of53
`
`CONFIDENTIAL
`
`PAGE 20 OF 53
`
`PROL0337667
`
`

`
`Data F11e D:\LIHsDATA\741901.D
`STD A
`
`Senple Name: 408705
`
`: 11/16/2015 9:42:11 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\741881.S
`lethod
`C: xmcutnxmu:1'uons\s294o:so2.n
`.
`.
`,
`DAD1 A. Sig-206.4 Re!-Zb0.1OO (741W1,D)
`
`MAU
`
`Z0
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : S n1
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ __ __' _ _ _ _ _ __| _ _ _ _ _ _ _ _ __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.663 PB
`0.2676 4016.40112 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`G016.40112
`
`Result: nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/16/2015 9:55:03 PH GT
`
`Page lot 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/20l6,
`page2lof53
`
`CONFIDENTIAL
`
`PAGE 21 OF 53
`
`PROL0337668
`
`

`
`Data File D:\l.IHSOATA\742200.D
`IllilllllllllllllIIIIIIIllIIIIIlllllllllllImllIIIIIIIIIIIIIIIIIIIIIII
`Iniection Date
`11/17/2015 6:12:16 Pl!
`Sea. Line :
`1
`$991: Male
`408677
`Locecion : V1.91 1
`Ace. Oneracor
`GT
`In1 :
`1
`Aca. Insuulent
`Inscrunenc 1
`In) Volune : S 111
`Sequence F11e
`D: \LIHSDATA\742199. S
`lechod
`C: \HPCHEH\ l\HITHODS\62940t502 .H
`.
`.
`.
`
`.uuuuuu
`
`DAD1 A. sq-2oa.4 ea-3oo.1oo'(7422oo.o)
`
`Suple Nunez 408677
`
`150
`
`1%
`
`:s:::::::::::=::u::n::::=:332:x:3::=:uan=:ax::::n:::::u::::::::n::x::
`Area PQKCCYIC RCDOIXC
`nun-nun-:-----an-n----u--Inunn-nansnnnn-unsun---nun:-3--I--a--n--an-I
`
`sicmal
`:
`sorted Bv
`11/16/2015 2:21:49 PH
`Ca11b. Data loditxed :
`1.0000
`luluoliez
`:
`1 . 0000
`Diluczon
`'
`Use Hulupliez 5. Dilution Factor Inth ISTD:
`
`Signal 1: DAN. A, 519-266,‘! Re!-360,100
`Nae
`Area
`Peak RetTiIe ‘Noe
`lhdth
`Area
`=1:
`I
`[min]
`r um f|AU*:1
`—--—l ----- --I ---- --4 ----- --I -------- -—| ------- -—a ------------------- --
`1
`8.100
`0.0000
`0.00000
`0.0000 Bzontenec
`
`Totals :
`
`0.00000
`
`Results obtained with enhanced integrator‘
`1 Uazninq: or Errors :
`
`llezninq : Canbrated conpound(:) not round
`nn--nun-:annInn:-nnunInnInunnannnnxx:nnnu:nu:nnnunnnnxnnxnnxxxxn-nun:
`*" End 02 Report "*
`
`Insczunent 1 11/17/2015 6:25:09 PH 61‘
`
`P190 1 91 1
`
`( Vpronmlographic Dalafrom the Stability I-.'ra/nation nfBrong/lmnc Sodium Drug Producl Samples _/hr l’oIwx'_\'. I/I2/20l6,
`page 22 of 53
`
`CONFIDENTIAL
`
`PAGE 22 OF 53
`
`PROL0337669
`
`

`
`Dace F11e D:\l.IHSDATA\742201.D
`nllannnnnncnlllnnlullItIInIIInuIn::1II21::nu:llnunlnulnnsxnnunnsnnlln
`Iniection Date
`11/17/2015 6:27:04 Pl!
`Sea. Line :
`2
`Supple Hue
`408677
`Locecion : V191 1
`Ace. Oneracor
`GT
`In1 :
`1
`Aca. Insuulent
`Inscrunenc 1
`In) Volune : S 111
`Sequence F11e
`D: \LIHSDATA\742199. S
`lechod
`C: \HPCHEH\ l\HITHODS\62940t502 .H
`.
`.
`.
`
`.uuuuuu
`
`DAD1 A. s..-2oo.4 ea-3oo.1oo'(7422o1.o)
`
`Suple Nunez 408677
`
`150
`
`1%
`
`:s:::::::::::=::u::n::::=:332:x:3::=:uan=:ax::::n:::::u::::::::n::x::
`Area PQKCCYIC RCDOIXC
`nun-nun-:-----an-n----u--Inunn-nansnnnn-unsun---nun:-3--I--a--n--an-I
`
`sicmal
`:
`sorted Bv
`11/16/2015 2:21:49 PH
`Calib. Data loditxed :
`1.0000
`luluoliez
`:
`1 . 0000
`Diluczon
`'
`Use Hultxpliez 5. Dilution Factor Inth ISTD:
`
`Signal 1: DAN. A, 519-266,‘! Re!-360,100
`Nae
`Area
`Peak RetTiIe ‘Noe
`lhdth
`Area
`=1:
`I
`[min]
`r um f|AU*:1
`—--—l ----- --I ---- --4 ----- --I -------- -—| ------- --1 ------------------- --
`1
`8.100
`0.0000
`0.00000
`0.0000 Bzontenec
`
`Totals :
`
`0.00000
`
`Results obtained with enhanced integrator‘
`1 Uazninq: or Errors :
`
`llezninq : Canbrated conpound(:) not round
`nn--nun-:annInn:-nnunInnInunnannnnxx:nnnu:nu:nnnunnnnxnnxnnxxxxn-nun:
`*" End 02 Report "*
`
`Insczunent 1 11/17/2015 6:39:55 PH 61‘
`
`P190 1 91 1
`
`( Vpronmlographic Dalafrom the Stability I-.'ra/nation nfBrong/lmnc Sodium Drug Producl Samples _/hr l’oIwx'_\'. I/I2/2016,
`page 23 M53
`
`CONFIDENTIAL
`
`PAGE 23 OF 53
`
`PROL0337670
`
`

`
`Data File D:\LIH$DATA\'M2ZD2.D
`
`
`
`
`Sanple liane: 408705
`
`
`
`
`
`Extended
`
`Instrument:
`Instrument 1
`
`
`
`
`
`rertornsnce Report
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`nodule
`Firmware revision Serial number
`
`
`
`
`
`__________________________________ __I___-_.-____________|_____-_________
`1100 Ouaternerv Puma
`.I..05..I.1 F0131
`11370201400
`
`
`
`
`
`
`
`
`1100 Autoselfller
`.\.D5..Ll
`|'D13'|
`US'?|32D1352
`
`
`
`
`
`
`
`1.100 Diode Arrev Detector
`1.05.11 F0131
`l.FS6ddl3|3691
`
`
`
`
`
`
`
`
`DE6306415B
`11.00 Coluln Therlostat
`5.05.11 [013]
`
`
`
`
`
`
`
`
`Software Revision: RGO’. 1.10.02 [1757] Compriqht G Afiilent Technologies
`
`
`
`
`
`
`
`
`
`
`
`
`Coluan Destrintion : Shiseido Cancel]. Pal: C18
`
`
`
`
`
`
`Product!
`Baitchl‘:
`:
`12503
`
`Serial!
`: M013 M232
`
`
`2.1 II
`Diameter
`:
`
`5.0 no
`Particle size
`:
`
`
`
`
`400 bar
`Haximun Pressure
`:
`
`
`
`
`
`0 ‘C
`Haxiuun Tennerature:
`
`
`
`
`Content
`: LIBS 405201
`
`
`
`
`
`100.0 II
`
`68.0 %
`11
`
`
`
`
`
`Lennrth :
`
`Void volume :
`
`
`llaxinun pl-I
`:
`
`
`
`
`
`
`
`
`
`
`
`l3:\I'IPCI'llZll\1\HE1'li0'DS\62l94fl5D1.K
`Analysis nethod:
`
`
`
`
`
`Samnle intonation tor Location:
`
`
`
`Saunle Ilene:
`400105
`
`
`
`Iniectionl:
`J.
`
`
`5 ul
`Injection volune:
`
`
`
`Acquisition intonation:
`
`
`
`
`
`1.00
`1.00
`
`
`
`
`
`Eultiolier:
`Dilution:
`
`
`
`
`
`Via]. 2
`
`
`
`
`
`
`Uoerator:
`GT
`
`
`1JJJ.7.r'2D15 6:42:06 Pl!
`Dateffile:
`
`
`
`
`D:\LIfi5M.T£\‘J42202.D
`Date tile nale:
`
`
`
`
`Itethod tile nane: C:\I-IPCI-I!.'H\1\H£‘1'I-I01)$\62'.940501.!*l
`
`
`
`
`
`
`
`1.500
`nlfnin
`flow:
`
`
`
`
`Pressure at end:
`115 bar
`Pressure at start:
`
`
`
`
`
`
`
`Luett Team. at end:
`2S.1‘C
`Lett Tenn. at start:
`
`
`
`
`
`
`
`
`
`Right ‘Tenp. at end:
`Right Tenp. at start: 25.1'l3
`
`
`
`
`
`
`
`
`
`Solvents:
`FHPI. Solvent A6204-05-01 {exp 1Z!l6)'15)
`
`
`
`
`
`
`PHP1. Solvent 3
`
`
`
`PHI-'1. Solvent 0
`
`
`
`MP1, Solvent D
`
`
`
`
`
`
`
`
`117 bar
`
`25.0 '0
`
`
`25.0 ‘C
`
`
`
`
`
`Signal description: DAD1 L, Sic-v266,4 Re:-660,100
`
`
`
`
`
`
`
`
`Instrument 1 1.'|J1'U2E|15 6:54:59 PH 61'
`
`
`
`
`
`
`
`Page J. oi «I
`
`Chrorraatagruphfc Datafrom the Srabihry Emfuarion ofBr'omfem:c Sodfrrm Drug Product Sampfearfor Potency, l!12!20 16,
`
`
`
`
`
`
`
`
`
`
`
`
`
`page 24 of53
`
`
`
`
`
`CONFIDENTIAL
`
`
`
`PAGE 24 OF 53
`
`PROL0337671
`
`
`
`PAGE 24 OF 53
`
`

`
`Dace rue D:\LnlSDA1'A\742202.D
`DAD1 A. Sif2@.4 RQIIVAW (732202 0)
`
`Suple Ilene: 408705
`
`
`
`Insuunent 1 11/17/2015 6:54:59 PH 61'
`
`up 2 ol 4
`
`Chrmnulographic Datafrom the Stability I'.'mfuaIi0n cgfliromfenarr Sodium Drug Pzlmlllcl Salnplcs jbr Polencjr, I/I2/20I 6,
`page 25 of 53
`
`CONFIDENTIAL
`
`PAGE 25 OF 53
`
`PROL0337672
`
`

`
`Data F11: D:\LnlsDA1‘A\742202.D
`Conoundl 1
`: Bzontenac
`Anount( nq/nu): 0.0000
`
`Sample line: 408705
`
`Peak description mm:
`Sumol: DAD1 A, 51¢-266.4 Re!-360.100
`RetTne: 8.669
`k‘:
`54.210
`Hnoht:
`229.20
`Area:
`4011.8
`Start:
`8.372
`End:
`10.001
`Skeu:
`0.937
`Excess:
`2.020
`llxdth at halt hemht:
`0.267
`5 none:
`0.587
`tanaent:
`0.476
`taxnnq:
`0.573
`Svlletlvz
`0.453
`USP Tuhnu:
`1.776
`Inteazatxon tvbe:
`33
`‘hit xnczcnnt (Inc):
`400.0
`Data pomts:
`282
`
`
`
`Statxaucu nonents (83 peak detectxon):
`H0:
`4009.1
`111:
`8.741
`Tanaent method
`52:
`0.016406
`Heltlndth nethod
`H3:
`0.001969
`5 sun: nethod
`114:
`0.001351
`Stctxstxcol
`
`Etncxcncvz Plates nu:
`colunn
`5297
`5855
`5459
`4658
`
`..
`nete:
`52973
`58546
`$4587
`46575
`
`Relatxonshm to preceedma beak:
`Resolutxon Tanaent Iethod:
`Ihltuxdth method
`
`-
`-
`
`Selectxvxtv:
`S stun method
`Steustical nethod
`
`-
`-
`-
`
`Instrument 1 11/17/2015 6:54:59 P)! G1‘
`
`in. a 0! 4
`
`(Wromalographic Datafrom Ihe Slabiliry l'.'\'aIuaIion ofBromfvnac Sodium Dnlg I’rodu¢'I Samples for Polencjr, II I 2/20| 6,
`page 26 of 574
`
`CONFIDENTIAL
`
`PAGE 26 OF 53
`
`PROL0337673
`
`

`
`Data rue D:\l.IlISDATA\742202.D
`I Ret.Tne
`Anount
`lnml
`Ina/ull
`
`1'"" 3.669‘
`Total:
`
`0.0000‘
`0.0000
`
`lane
`
`Pace
`I
`
`a:on:enac"
`
`3
`
`-'- End 0! Report -'1
`
`Se-pie Ilene: 408705
`
`Inscrunenr. 1 11/17/2015 6:54:59 PH GT
`
`up 0 ol 1
`
`( 'hr0muIograpIu'c I)aIafrom the Slnhilily I'.'\'nIuaIion Q/‘Iirom/i'nac Sodium Drug I’roducI Samples jbr I’vIenc_r. I.’ I 2/20l 6,
`page 27 M53
`
`CONFIDENTIAL
`
`PAGE 27 OF 53
`
`PROLO337674
`
`

`
`Data File D:\LIHsDATA\742Z03.D
`STD A
`
`Senple Name: 408705
`
`: 11/17/2015 6:57:19 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\742199.S
`lethod
`c:xupcutnx1\nt1nons\s294oso2.n
`.
`.
`,
`DAD1 A. Sig-206.4 Re!-150.100 (7422030)
`
`MAU
`
`4
`Sea. Line :
`Locet1on : V101 2
`In1 :
`1
`Inj Volune : S n1
`
`150
`
`100
`
`I-nuan-nun-anus:-n-3-nuunznznnnnnnnnansuz-nun:--z-nsunsununu:-:2-an-u
`Area Percent Renort
`Inn:-nun-nnxnnnnnnnnnnnnnuns:anI:2:32:nnnxxmnannnnnnssnnnxnxannnnnnnx
`
`siunol
`:
`Sorted BV
`11/16/2015 2:21:49 PH
`Cohb. Data Hoditied :
`1.0000
`lultiblier
`:
`1.0000
`Dxlutzon
`:
`Use Hu1t1p11er c. Duutton Factor uath ISTDs
`
`Signal 1: DAD1 A, Sig-266,4 Ret=360,100
`Area
`Peak RetTne ‘Noe
`Hxdth
`Area
`&
`!
`rnznl
`fnznl
`rIAU*s1
`-___| _ _ _ _ _ __| _ _ _ _ __' _ _ _ _ — __| _ _ _ _ _ _ _ _ __| _ _ _ _ .- _ __' _ __ _ — _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
`1
`8.670 B?
`0.2665 4013.03003 100.0000 Brontenec
`
`Nam.-
`
`Totals :
`
`G013.03003
`
`Result: nbtuned uuzh enhanced xntegrator!
`1 Burning: or Errors :
`
`llarmnq : Invalid cahbrauon curve,
`
`(Bronhenac)
`
`**' End of Report
`
`'*'
`
`Instrument 1 11/17/2015 7:10:10 PH GT
`
`:19. lot 1
`
`Chromatographic Dalafrom the Stability I:'ra/Marion nfBromjknm- Sodium Drug Producl Samples for PoIwx'_I'. I/I2/2016,
`page28of53
`
`CONFIDENTIAL
`
`PAGE 28 OF 53
`
`PROL0337675
`
`

`
`Data File D:\LIHsDATA\742204.D
`STD A
`
`Senple Name: 408705
`
`: 11/17/2015 7:12:05 PH
`In1ect1on Date
`: 403705
`sannle Rene
`: GT
`Ace. Operator
`Aca. Instrunent :
`Instrument 1
`Secmence File
`D:\LIHSDATA\742199.S
`lethod
`C:\HPcH£H\1\HITHODs\62940502.H
`.
`.
`,
`DAD1 A. Sig-206.4 Re!-ZbO.100 (7422040)
`
`MAU
`
`5
`Sea. Line