,. 55(]'"
`-
`~ ~ A Division of Albany Molecular Research Inc.
`
`3065 Kent Avenue
`West Lafayette, IN 47906-1076
`Phone : (765) 463-0112
`Fax : (765) 463-4722
`E-mail: info@ssci-inc.com
`Web: www.ssci-inc.com
`
`Chromatographic Data from
`the Stability Evaluation of
`Bromfenac Sodium Drug
`Product Samples for Potency
`
`Project ID: EL20151326
`Report Date: 1112/2016
`
`CONFIDENTIAL
`
`PROL0337648
`
`PAGE 1 OF 53
`
`SENJU EXHIBIT 2266
`LUPIN v. SENJU
`IPR2015-01105
`
`
`-
`~ ~ A Division of Albany Molecular Research Inc.
`
`3065 Kent Avenue
`West Lafayette, IN 47906-1076
`Phone : (765) 463-0112
`Fax : (765) 463-4722
`E-mail: info@ssci-inc.com
`Web: www.ssci-inc.com
`
`Chromatographic Data from
`the Stability Evaluation of
`Bromfenac Sodium Drug
`Product Samples for Potency
`
`Project ID: EL20151326
`Report Date: 1112/2016
`
`CONFIDENTIAL
`
`PROL0337648
`
`PAGE 1 OF 53
`
`SENJU EXHIBIT 2266
`LUPIN v. SENJU
`IPR2015-01105
`
`
`
`I. SUMMARY
`
`This document contains chromatographic stability da ta from the analysis of Bromfenac sodium
`ophthalmic solution drug product for potency . Samples were sourced from cnJu.
`
`Table I. Summary of HPLC Data, Sequence 741881
`
`Sample
`Description
`Blank
`Blank
`STDA
`STDA
`STDA
`STDA
`STDA
`STD B
`Blank
`STDA
`240031
`240031
`240031
`STDA
`
`LIMS LC F en a me
`
`RT
`
`Area(mAU*s)
`
`Page
`
`408677
`408677
`408705
`408705
`408705
`408705
`408705
`408706
`408677
`408705
`403486
`403489
`403490
`408705
`
`741882
`741883
`741884
`741885
`741886
`741887
`741888
`741889
`741890
`741897
`741898
`741899
`741900
`741901
`
`---
`---
`8.667
`8.668
`8.666
`8.666
`8.666
`8.665
`---
`8.666
`8.646
`8.648
`8.647
`8.663
`
`---
`---
`4012.66
`4015.13
`4016.96
`4016.04
`4018.79
`4038.45
`---
`4019.73
`4556.16
`4548.27
`4547.03
`4016.40
`
`5
`6
`7
`11
`12
`13
`14
`15
`16
`17
`18
`19
`20
`21
`
`hroma/Ographic Datafi'omlhe Stability Eva/ualion ofBromfenac Sodium Dmg Producl Samples for Potency, 1/ 12120 16,
`page 2 of 53
`
`CONFIDENTIAL
`
`PROL0337649
`
`PAGE 2 OF 53
`
`
`
`Table 2. Summary of HPLC Data, Sequence
`
`Sample
`Description
`Blank
`Blank
`STDA
`STDA
`STDA
`STDA
`STDA
`STD B
`Blank
`STDA
`STDA
`STDA
`STDA
`STDA
`STDA
`STDA
`STDA
`240031
`240031
`240031
`240031
`240031
`240031
`STDA
`240031
`240031
`240031
`240031
`STDA
`
`LIMS LC F en a me
`
`408677
`408677
`408705
`408705
`408705
`408705
`408705
`408706
`408677
`408705
`408705
`408705
`408705
`408705
`408705
`408705
`408705
`403478
`403479
`403480
`403481
`403482
`403483
`408705
`403484
`403485
`403487
`403488
`408705
`
`742200
`742201
`742202
`742203
`742204
`742205
`742206
`742207
`742208
`742215
`742222
`742229
`742235
`742242
`742249
`742256
`742262
`742263
`742264
`742265
`742266
`742267
`742268
`742269
`742272
`742273
`742274
`742275
`742276
`
`RT
`---
`---
`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
`
`Area(mAU*s)
`---
`---
`4011.82
`4013.03
`4010.89
`4010.87
`4015.36
`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
`4556.05
`4024.68
`4541.95
`4541.17
`4524.65
`4523.19
`4024.02
`
`Page
`
`22
`23
`24
`28
`29
`30
`31
`32
`33
`34
`35
`36
`37
`38
`39
`40
`41
`42
`43
`44
`45
`46
`47
`48
`49
`50
`51
`52
`53
`
`hroma/Ographic Datafi'omlhe Stability Eva/ualion ofBromfenac Sodium Drug Producl Samples for Potency, 1/ 1212016,
`page 3 of 53
`
`CONFIDENTIAL
`
`PROL0337650
`
`PAGE 3 OF 53
`
`
`
`II. CHROMA TOG RAMS
`
`hroma/Ographic Datafi"omlhe Stability Eva/ualion ofBromfenac Sodium Drug Product Samples for Polency, 1/1212016,
`page 4 of 53
`
`CONFIDENTIAL
`
`PROL0337651
`
`PAGE 4 OF 53
`
`
`
`Daca File D: \LIHSDATA\7 41882. 0
`
`Saaple Naae: 408677
`
`11/ 16/2015 5:01:26 PM
`Iniec~ion Da~e
`408677
`Saaole Naae
`GT
`Aca. Ooeracor
`Instrument 1
`Aca. Instrument
`Seauence File
`D:\LIMSDATA\741881.5
`Method
`C: \HPCHEM\ 1 \ IIETHODS\62940!502. M
`ll / 16/201 5 3:25:25 PH hv GT
`Lft~r. chMHt~d
`DAD1 A. Sig•2ee.4 Rof-31S0.100 (741882.0)
`
`Sea. Line
`Location
`Ini
`Inj Volwoe
`
`1
`Vial
`1
`5 111
`
`mAU
`
`250
`
`200
`
`150
`
`100
`
`50
`
`0
`
`r.
`
`?
`
`4
`
`1n
`
`Area Percent Reoor rt
`
`Sianal
`sorted Bv
`11/16/2015
`Calib. Data Modified
`1. 0000
`Mul tiolier
`1. 0000
`Dilution
`Use Multiplier & Dilution Factor with ISTDs
`
`2:21:49 PM
`
`Si gnal 1: DAD! A, Si q•266,4 Ref=360,100
`
`IJidth
`Area
`Aro!a
`Nue
`Peel< RetTbe Tvoe
`r .. inl
`rmAu•sl
`''
`rminl
`1
`---- l-------l------1------- l---------- l----·----l---------------------
`l
`8. 100
`0 . 0000
`0.00000
`0 . 0000 Bromfenac
`
`Total s
`
`0.00000
`
`Resu lts obtained with enhanced inteqracor 1
`1 tJarninqs or Errors
`
`IJarninq : Calibrated co .. pound(s) not found
`
`••• End of Report •••
`
`Instrument 1 11/16/2015 5: 14: 25 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 5 of 53
`
`CONFIDENTIAL
`
`PROL0337652
`
`PAGE 5 OF 53
`
`
`
`Daca File D: \LIHSDATA\7 41883. 0
`
`Saaple Naae: 408677
`
`11/ 16/2015 5:16:11 PM
`Iniec~ion Da~e
`408677
`Saaole Naae
`GT
`Aca. Ooeracor
`Instrument 1
`Aca. Instrument
`Seauence File
`D:\LIMSDATA\741881.5
`Method
`C: \HPCHEM\ 1 \ IIETHODS\62940!502. M
`ll / 16/201 5 3:25:25 PH hv GT
`Lft~r. chMHt~d
`DAD1 A. Sig•2ee.4 Rof-31S0.100 (741883.0)
`
`Sea. Line
`Location
`Ini
`Inj Volwoe
`
`2
`Vial
`1
`5 111
`
`mAU
`
`250
`
`200
`
`150
`
`100
`
`50
`
`0
`
`r.
`
`?
`
`4
`
`1n
`
`Area Percent Reoor rt
`
`Sianal
`sorted Bv
`11/16/2015
`Calib. Data Modified
`1. 0000
`Mul tiolier
`1. 0000
`Dilution
`Use Multiplier & Dilution Factor with ISTDs
`
`2:21:49 PM
`
`Si gnal 1: DAD! A, Si q•266,4 Ref=360,100
`
`IJidth
`Area
`Aro!a
`Nue
`Peel< RetTbe Tvoe
`r .. inl
`rmAu•sl
`''
`rminl
`1
`----l-------l------1------- l---------- l----·----l---------------------
`l
`8. 100
`0 . 0000
`0.00000
`0 . 0000 Bromfenac
`
`Total s
`
`0.00000
`
`Resu lts obtained with enhanced inteqracor 1
`1 tJarninqs or Errors
`
`IJarninq : Calibrated co .. pound(s) not found
`
`••• End of Report •••
`
`Instrument 1 11/16/2015 5:29:10 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 6 of 53
`
`CONFIDENTIAL
`
`PROL0337653
`
`PAGE 6 OF 53
`
`
`
`Daca File D: \LIHSDATA\741884. 0
`
`Sample Naae: 408705
`
`E xcended
`
`P e r t o r m a n c e
`
`R e p o r c
`
`Instrument: Instrument 1
`
`Module
`Firm•11ue revision Setial nu.m.bet
`------------------------------------l-----·-------------l---------------
`A.05 • .ll r0131
`1100 ()uatetnarv Pump
`US70201400
`A.05 . .ll r 0131
`1100 Autosaapler
`US70201352
`A.05 • .ll r ol31
`1100 Diode Anav Detector
`US64400691
`A.05 • .ll [ 013]
`1100 COlUIIUl Thermostac
`D£63064158
`
`Software Revision: Rev . A. l0.02 (1757] Cop~iriqht ~ Aqilent Technoloqies
`
`Column DescriPtion
`Product#
`Seria U'
`Diueter
`Patticle size
`:
`Maximum Pressure
`Maximum Temperature:
`Couent
`
`Shiseido Capce11
`12503
`AAAB 07232
`2 .1 IIUl
`5.0 \.Ul
`400 bar
`o ·c
`LIMS 405201
`
`Pak Cl 8
`Batcchl:
`
`Lenolth
`Void VO!l.lllle
`Maximum 1tH
`
`100. 0 llll
`68.0
`,Q
`
`Analysis method:
`
`C: \HPCHEM\1 \METHODS\62:940501. II
`
`Sample information tor Location:
`
`Vial 2
`
`408705
`Sup1e Na»e:
`1
`I niectionl:
`Injection volume: 5 ~1
`
`Acquisition intotmati on:
`
`llultiplier:
`Dilution:
`
`1. 00
`1. 00
`
`Operator:
`GT
`ll/ 16/2015 5 : 31 :14 PM
`Date/Time:
`D: \L IMSDATA\741884.D
`Data file name:
`Method file name: C: \HPCHEM\ 1 \METHODS\62:9 40501. II
`
`n ow:
`Pressure at start:
`Left Temp. at start:
`Right Temp. at start:
`
`1. 500 ml/min
`115 bat
`25.l "C
`25. 0 "C
`
`Pressure at end:
`L•e ft Temp. at end:
`Right Temp. at end:
`
`117 bar,
`25.1 ·c
`25. 0
`· c
`
`Solvencs:
`
`PI!Pl, Solvent A 62'94-05-01 (exp 12/16/15)
`PMPl, Sol vent B
`PI!Pl, Sol vent C
`PMPl, Solvent D
`
`Siqnal description: DAD! A, Siq=266,4 Ref••360 , 100
`
`Instrument 1 11/16/2015 5: 44:14 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 7 of 53
`
`CONFIDENTIAL
`
`PROL0337654
`
`PAGE 7 OF 53
`
`
`
`Data rile D:\LIMSDATA\741884.0
`
`Sample Name: 408705
`
`DAD1 A. Sig•266.4 Rot-3l!0 .100 (741884.0)
`
`mAU
`
`200
`
`100
`
`2
`
`4
`
`10
`
`12
`
`rni
`
`Inst~ument l 11/16/2015 5:44:14 PH GT
`
`hromalographic Dalafrom the Stability Eva/ualion ofBromfenac Sodium Drug Product Samples for Potency, 1112/2016,
`page 8 of 53
`
`CONFIDENTIAL
`
`PROL0337655
`
`PAGE 8 OF 53
`
`
`
`Date. rile D: \LIMSDATA\741884.0
`
`Sample Name: 408705
`
`200
`
`150
`
`100
`
`: Bromfenac
`Comooundf 1
`Amount [ nq/u.l]: 0. 0000
`Peal< desctiDt.ion rIll in 1 :
`Sianal: DADl A, Siq~266,4 Ret~360,100 r-::-:-::-r----,r-----------,
`k I;
`RetTime: 8 .667
`54.199
`mAU
`HeiClht.:
`228.15
`Area:
`4012.7
`St.e.rt.:
`8.365
`End:
`9.952
`0.888
`1. 577
`Skew:
`Excess:
`0.270
`Uidth at. half heiCJht:
`5 si(JIIIa :
`0.587
`0.478
`te.nCJent:
`te.ilinq :
`0.573
`0.454
`l. 771
`BB
`400.0
`274
`
`Svuetrv:
`USP Te.ilinu:
`Inteurat.ion tvoe:
`Time increment [msec) :
`Data points:
`
`50
`
`0
`
`Statistical moments
`40U.8
`MO:
`Ml:
`8. 738
`M2:
`0. 016448
`0. 001874
`M3:
`M4:
`0. 001238
`
`(BB peak detection):
`
`Te.nqent. method
`He.lfwidth method
`5 siC!Iaa method
`Statistical
`
`Efficiency: Pl ates
`column
`5251
`5709
`5457
`4642
`
`oer ..
`meter
`52510
`57088
`54566
`46423
`
`Rel ationshiP to oreceedinu oee.k:
`Resolution Te.nuent method:
`Haltwidth method
`
`Se l ectilli tv:
`5 s:i.(JIIIa method
`Statistical method
`
`Instrument 1 ll/16/2015 5:44:14 PH GT
`
`hromalographic Dalafrom the Stability Eva/ualion ofBromfenac Sodium Drug Product Samples for Potency, 1112/20 16,
`page 9 of 53
`
`CONFIDENTIAL
`
`PROL0337656
`
`PAGE 9 OF 53
`
`
`
`Daca File D: \LIMSDATA\741884.0
`
`Sample Name: 408705
`
`I
`
`Rec. Time
`[minl
`
`8.667
`
`Total:
`
`Amo~mc
`rncr/ull
`o.oooo(cid:173)
`o.oooo
`
`Btomfenac-
`
`••• End of Repotc •••
`
`Name Paae
`
`'
`
`3
`
`Inst~ument l ll/16/2015 5:44:14 PH GT
`
`Pillge 4 of 4
`
`hroma/Ographic Data from the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/ 12120 16,
`page 10 of 53
`
`CONFIDENTIAL
`
`PROL0337657
`
`PAGE 10 OF 53
`
`
`
`Daca File D:\LIHSDATA\741885.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/16/2015 5:46:26 PM
`Iniection Dace
`408705
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (741885.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`4
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorced Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilucion
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`---- l-------l------l------- l----------1----··--- l---------------------
`l
`8.668 BB
`0 . 2694 4015.13452 100 . 0000 Bromfenac
`
`Tota l ~
`
`4015.13452
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 5:59: 25 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 11 of 53
`
`CONFIDENTIAL
`
`PROL0337658
`
`PAGE 11 OF 53
`
`
`
`Daca File D:\LIHSDATA\741886.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/16/2015 6:01:13 PM
`Iniection Dace
`408705
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\62940!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (7418Se.l>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`5
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Repor rc
`
`Sianal
`sorced Bv
`11/16!2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilucion
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rminl
`rllAU•sl
`:;
`I
`----1-------l------l-------l----------l----··--- l---------------------
`l
`8.666 PP
`0 . 2674 4016.96460 100 . 0000 Bromfenac
`
`Tota l ~
`
`4016.96460
`
`Result~ obtained with enhanced integracor !
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 6:14: 11 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 12 of 53
`
`CONFIDENTIAL
`
`PROL0337659
`
`PAGE 12 OF 53
`
`
`
`Daca File D:\LIHSDATA\741887.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/16/2015 6:15:57 PM
`Iniection Dace
`408705
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (741887.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`6
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorced Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilucion
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`---- l-------l------l------- l----------1----··--- l---------------------
`l
`8.666 BB
`0 . 2675 4016.03931 100 . 0000 Bromfenac
`
`Tota l ~
`
`4016.03931
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 6:28:55 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 13 of 53
`
`CONFIDENTIAL
`
`PROL0337660
`
`PAGE 13 OF 53
`
`
`
`Daca File D: \LIHSDATA\7 4l888. D
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/16/2015 6:30: 41 PM
`Iniection Dace
`Sample Name
`408705
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (741888.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`7
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorted Bv
`ll/16/2015 2:21:49 PM
`Calib. Daca Modified
`Mulciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266, 4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rminl
`rllAU•sl
`:;
`I
`---- l-------l------l------- l----------1----··--- l---------------------
`l
`8. 666 BP
`0 . 2695 4018.79224 100 . 0000 Bromfenac
`
`Tota l ~
`
`4018.79224
`
`Result~ obtained with enhanced integracor !
`1 Warnings or Errors :
`
`Warning : Invalid calibrati on curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 6:43:40 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 14 of 53
`
`CONFIDENTIAL
`
`PROL0337661
`
`PAGE 14 OF 53
`
`
`
`Daca File D:\LIHSDATA\74l889.D
`
`STI> B
`
`Sa.ple Name: 408706
`
`ll/16/2015 6:45:24 PM
`Iniection Dace
`408706
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (7418SQ.I>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`8
`Vial 3
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorted Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`----1-------l------l------- l----------l----··--- l---------------------
`l
`8.665 PB
`0 . 2677 4038.44849 100 . 0000 Bromfenac
`
`Tota l ~
`
`4038.44849
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 6:58:24 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 15 of 53
`
`CONFIDENTIAL
`
`PROL0337662
`
`PAGE 15 OF 53
`
`
`
`Daca File D: \LIHSDATA\7 41890 . 0
`
`Saaple Naae: 408677
`
`11/ 16/2015 7:00:09 PM
`Iniec~ion Da~e
`408677
`Saaole Naae
`GT
`Aca. Ooeracor
`Instrument 1
`Aca. Instrument
`Seauence File
`D:\LI MSDATA\741881.5
`Method
`C: \HPCHEM\ 1 \ IIETHODS\629 40!502. M
`ll / 16/201 5 3:25:25 PH hv GT
`Lft~r. chMHt~d
`DAD1 A. Sig•2ee.4 Rof-31S0.100 (741800.0)
`
`Sea. Line
`Location
`Ini
`Inj Volwoe
`
`9
`Vial
`1
`5 111
`
`mAU
`
`250
`
`200
`
`150
`
`100
`
`50
`
`0
`
`r.
`
`?
`
`4
`
`1n
`
`Area Percent Reoorrt
`
`Sianal
`sorted Bv
`11/16/2015
`Cal ib. Data Modified
`1. 0000
`Mul tiolier
`1. 0000
`Dilution
`Use Mu l tiplier & Diluti on Factor with ISTDs
`
`2:21 :49 PM
`
`Si gnal 1: DAD! A, Si q•266,4 Ref=360,100
`
`Peel< RetTbe Tvoe
`IJidth
`Area
`Aro!a
`Nue
`rminl
`r .. inl
`rmAu•sl
`''
`1
`---- l-------l------ 1------- l---------- l----·----l---------------------
`l
`8. 100
`0 . 0000
`0.00000
`0 . 0000 Bromfenac
`
`Total s
`
`0.00000
`
`Resu l ts obtained with enhanced inteqracor 1
`1 tJarninqs or Errors
`
`IJarninq : Calibrated co .. pound(s) not found
`
`• •• End of Report • ••
`
`Instrument 1 11/16/2015 7: 13: 07 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 16of53
`
`CONFIDENTIAL
`
`PROL0337663
`
`PAGE 16 OF 53
`
`
`
`Daca File D:\LIHSDATA\741897.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/16/2015 8:43:13 PM
`Iniection Dace
`408705
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (7418il7.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`16
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Repor rc
`
`Sianal
`sorced Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilucion
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`---- l-------l------l------- l----------1----··--- l---------------------
`l
`8.666 PP
`0 . 2677 4019.73315 100 . 0000 Bromfenac
`
`Tota l ~
`
`4019.73315
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 8:56:11 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 17 of 53
`
`CONFIDENTIAL
`
`PROL0337664
`
`PAGE 17 OF 53
`
`
`
`Daca File D:\LIHSDATA\74l898.D
`
`240031
`
`Sa.ple Name: 403486
`
`ll/16/2015 8:57:59 PM
`Iniection Dace
`403486
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (7418il8.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`17
`Vial 10
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorted Bv
`11/16!2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTDs
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`----1-------l------l------- l----------l----··--- l---------------------
`l
`8.646 BP
`0 . 2741 4556.15869 100 . 0000 Bromfenac
`
`Tota l ~
`
`4556.15869
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 11!16!2015 9:10 :57 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 18of53
`
`CONFIDENTIAL
`
`PROL0337665
`
`PAGE 18 OF 53
`
`
`
`Daca File D:\LIHSDATA\74l899.D
`
`240031
`
`Sa.ple Name: 403489
`
`ll/16/2015 9:12:44 PM
`Iniection Dace
`403489
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (7418ilQ.I>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`18
`Vial 11
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorted Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTDs
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`---- l-------l------l------- l----------1----··--- l---------------------
`l
`8.648 PP
`0 . 2721 4548.27100 100 . 0000 Bromfenac
`
`Tota l ~
`
`4548.27100
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 ll/16/2015 9:25:41 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 19 of 53
`
`CONFIDENTIAL
`
`PROL0337666
`
`PAGE 19 OF 53
`
`
`
`Daca File D:\LIHSDATA\74l900.D
`
`240031
`
`Sa.ple Name: 403490
`
`ll/16/2015 9:27:27 PM
`Iniection Dace
`403490
`Sample Name
`Aca. Operacor
`GT
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\62940!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (741QOO.I>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`19
`Vial 12
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Repor rc
`
`Sianal
`sorted Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTDs
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rminl
`rllAU•sl
`:;
`I
`----1-------l------l-------l----------l----··--- l---------------------
`l
`8.647 PP
`0 . 2721 4547.03369 100 . 0000 Bromfenac
`
`Tota l ~
`
`4547.03369
`
`Result~ obtained with enhanced integracor !
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 ll/16/2015 9:40:24 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 20 of 53
`
`CONFIDENTIAL
`
`PROL0337667
`
`PAGE 20 OF 53
`
`
`
`Daca File D:\LIHSDATA\74l90l.D
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/16/2015 9:42:11 PM
`Iniection Dace
`408705
`Sample Name
`Aca. Operacor
`GT
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\74l88l.S
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\62940!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (741Q01 .1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`20
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorted Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rminl
`rllAU•sl
`:;
`I
`----l-------l------l-------l----------1----··--- l---------------------
`l
`8. 663 PB
`0 . 2676 4016.40112 100 . 0000 Bromfenac
`
`Tota l ~
`
`4016.40112
`
`Result~ obtained with enhanced integracor !
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 ll/16/2015 9:55:08 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 21 of 53
`
`CONFIDENTIAL
`
`PROL0337668
`
`PAGE 21 OF 53
`
`
`
`Daca File D:\LIHSDATA\742200.0
`
`Saaple Naae: 408677
`
`11/17/2015 6:12:16 PM
`Iniec~ion Da~e
`408677
`Saaole Naae
`GT
`Aca. Ooeracor
`Instrument 1
`Aca. Instrument
`Seauence File
`D:\LIMSDATA\742199.5
`Method
`C: \HPCHEM\ 1 \ IIETHODS\62940!502. M
`ll/16 /201 5 3:25:25 PH hv GT
`Lft~r. chMHt~d
`DAD1 A. Sig•2ee.4 Rof-31S0.100 (742200.0)
`
`Sea. Line
`Location
`Ini
`Inj Volwoe
`
`1
`Vial
`1
`5 111
`
`mAU
`
`250
`
`200
`
`150
`
`100
`
`50
`
`0
`
`r.
`
`?
`
`4
`
`1n
`
`Area Percent Reoorrt
`
`Sianal
`sorted Bv
`11/16/2015
`Calib. Data Modified
`1. 0000
`Mul tiolier
`1. 0000
`Dilution
`Use Multiplier & Dilution Factor with ISTDs
`
`2:21:49 PM
`
`Signal 1: DAD! A, Siq•266,4 Ref=360,100
`
`Peel< RetTbe Tvt>e
`IJidth
`Area
`Aro!a
`Nue
`rminl
`r .. inl
`rmAu•sl
`''
`1
`----l-------l------1------- l----------l----·----l---------------------
`l
`8. 100
`0 . 0000
`0.00000
`0 . 0000 Bromfenac
`
`Totals
`
`0.00000
`
`Results obtained with enhanced inteqracor 1
`1 tJarninqs or Errors
`
`IJarninq : Calibrated co .. pound(s) not found
`
`••• End of Report •••
`
`Instrument 1 11/17/2015 6:25: 09 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 22 of 53
`
`CONFIDENTIAL
`
`PROL0337669
`
`PAGE 22 OF 53
`
`
`
`Daca File D:\LIHSDATA\742201.0
`
`Saaple Naae: 408677
`
`11/17/2015 6:27:04 PM
`Iniec~ion Da~e
`408677
`Saaole Naae
`GT
`Aca. Ooeracor
`Instrument 1
`Aca. Instrument
`Seauence File
`D:\LIMSDATA\742199.5
`Method
`C: \HPCHEM\ 1 \ IIETHODS\62940!502. M
`ll/16 /201 5 3:25:25 PH hv GT
`Lft~r. chMHt~d
`DAD1 A. Sig•2ee.4 Rof-31S0.100(742201 .D)
`
`Sea. Line
`Location
`Ini
`Inj Volwoe
`
`2
`Vial
`1
`5 111
`
`mAU
`
`250
`
`200
`
`150
`
`100
`
`50
`
`0
`
`r.
`
`?
`
`4
`
`1n
`
`Area Percent Reoorrt
`
`Sianal
`sorted Bv
`11/16/2015
`Calib. Data Modified
`1. 0000
`Mul tiolier
`1. 0000
`Dilution
`Use Multiplier & Dilution Factor with ISTDs
`
`2:21:49 PM
`
`Signal 1: DAD! A, Siq•266,4 Ref=360,100
`
`Peel< RetTbe Tvt>e
`IJidth
`Area
`Aro!a
`Nue
`rminl
`r .. inl
`rmAu•sl
`''
`1
`----l-------l------1------- l----------l----·----l---------------------
`l
`8. 100
`0 . 0000
`0.00000
`0 . 0000 Bromfenac
`
`Totals
`
`0.00000
`
`Results obtained with enhanced inteqracor 1
`1 tJarninqs or Errors
`
`IJarninq : Calibrated co .. pound(s) not found
`
`••• End of Report •••
`
`Instrument 1 11/17/2015 6:39: 55 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 23 of 53
`
`CONFIDENTIAL
`
`PROL0337670
`
`PAGE 23 OF 53
`
`
`
`Daca File D: \LIHSDATA\74 2202. 0
`
`Sample Name: 408705
`
`E xcended
`
`P e r t o r m a n c e
`
`R e p o r c
`
`Instrument: Instrument 1
`
`Module
`Firm•11ue revision Setial nu.m.bet
`------------------------------------l-----·-------------l---------------
`A. OS • .ll r0131
`1100 ()uatetnarv Pump
`US70201400
`A. OS . .ll r 0131
`1100 Autosampler
`US702013S2
`A. OS • .ll r ol31
`1100 Diode Anav Detector
`US64400691
`A. OS • .ll [ 013]
`1100 COlUIIUl Thermostac
`D£63064158
`
`Software Revision: Rev . A. l0.02 (1757] Cop~iriqht ~ Aqilent Technoloqies
`
`Column DescriPtion
`Product#
`Seriall
`Diueter
`Patticle size
`:
`Maximum Pressure
`Maximum Temperature:
`Couent
`
`Shiseido Capce11
`12503
`AAAB 07232
`2 .1 IIUl
`s.o \.Ul
`400 bar
`o ·c
`LIMS 405201
`
`Pak Cl 8
`Batcchl:
`
`Lenolth
`Void VO!l.lllle
`Maximum 1tH
`
`100. 0 llll
`68.0
`,Q
`
`Analysis method:
`
`C: \HPCHEM\1 \METHODS\62:940501. II
`
`Sample information tor Location:
`
`Vial 2
`
`408705
`Sup1e Na»e:
`1
`I niectionl:
`Injection volume: 5 ~1
`
`Acquisition intotmati on:
`
`llultiplier:
`Dilution:
`
`1. 00
`1. 00
`
`Operator:
`GT
`ll/ 17/2015 6 :42:06 PM
`Date/Time:
`D: \L IMSDATA\742202.D
`Data file name:
`Method file name: C: \HPCHEM\ 1 \METHODS\62:9 40501. II
`
`n ow:
`Pressure at start:
`Left Temp. at start:
`Right Temp. at start:
`
`1. sao ml/min
`115 bat
`2S.l "C
`25.l"C
`
`Pressure at end:
`L•e ft Temp. at end:
`Right Temp. at end:
`
`117 bat
`2s. o ·c
`25. 0
`· c
`
`Solvencs:
`
`PI!Pl, Solvent A 62'94-05-01 (exp 12/16/15)
`PMPl, Sol vent B
`PI!Pl, Sol vent C
`PMPl, Solvent D
`
`Siqnal description: DAD! A, Siq=266,4 Ref••360 , 100
`
`Instrument 1 11/17/2015 6:54: 59 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 24 of 53
`
`CONFIDENTIAL
`
`PROL0337671
`
`PAGE 24 OF 53
`
`
`
`Data rile D:\LIMSDATA\742202.0
`
`Sample Name: 408705
`
`DAD1 A. Sig•266 .4 Rot-3l!0 .100 (742202.0)
`
`mAU
`
`200
`
`100
`
`2
`
`4
`
`10
`
`12
`
`rni
`
`Inst~ument l 11/17/2015 6:54:59 PH GT
`
`hromalographic Dalafrom the Stability Eva/ualion ofBromfenac Sodium Drug Product Samples for Potency, 1112/2016,
`page 25 of 53
`
`CONFIDENTIAL
`
`PROL0337672
`
`PAGE 25 OF 53
`
`
`
`Data rile D: \LIMSDATA\742202.0
`
`Sample Name: 408705
`
`: Bromfenac
`Comooundf 1
`Amount [ nq/u.l]: 0. 0000
`Peal< desctiDt.ion rIll in 1 :
`Si anal : DADl A, Siq~266 ,4 Ret~360,100
`RetTime: 8 . 669
`54.210
`k':
`HeiQht.:
`229 . 20
`Area:
`4011.8
`St.art.:
`8.372
`End:
`10.001
`Skew :
`0.937
`Excess :
`2.020
`Uidth at. half he:i.Qht:
`0.267
`5 si(JIDa :
`0.587
`tanQent:
`0.476
`tailinq:
`0.573
`0.453
`1. 776
`BB
`400. 0
`282
`
`Svuetrv:
`USP Tailinu:
`I nteurat.ion tvoe:
`Time incremen t [msec ) :
`Data poi nts:
`
`mAU
`
`--
`
`200
`
`150
`
`100
`
`50
`
`0
`
`J
`
`0
`
`Statistical moments
`4009.1
`MO:
`Ml :
`8. 741
`M2:
`0. 016406
`0.001969
`M3:
`M4:
`0. 001351
`
`(BB peal! det.ect.ion):
`
`Tanuent. method
`Halfwidth method
`5 siC!Iaa method
`Statistical
`
`Eff iciency: Pl ates
`column
`5297
`5855
`5459
`4658
`
`oer ..
`meter
`52973
`58546
`54587
`46575
`
`Rel ationshio to oreceedinu oeak:
`Resolution Tanuent method:
`Haltwidth method
`
`Se l ectilli tv:
`5 s:i.(JIDa method
`Statistical method
`
`Instrument l 11/17/2015 6:54:59 PH GT
`
`hromalographic Dalafrom the Stability Eva/ualion ofBromfenac Sodium Drug Product Samples for Potency, 1112/2016,
`page 26 of 53
`
`CONFIDENTIAL
`
`PROL0337673
`
`PAGE 26 OF 53
`
`
`
`Daca File D: \LIMSDATA\742202.0
`
`Sample Name: 408705
`
`I
`
`Rec. Time
`[minl
`
`8.669
`
`Total:
`
`Amo~mc
`rncr/ull
`o.oooo(cid:173)
`o.oooo
`
`Btomfenac-
`
`••• End of Repotc •••
`
`Name Paae
`
`'
`
`3
`
`Inst~ument l ll/17/2015 6:54:59 PH GT
`
`Pillge 4 of 4
`
`hroma/Ographic Data from the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency , 1/ 12120 16,
`page 27 of 53
`
`CONFIDENTIAL
`
`PROL0337674
`
`PAGE 27 OF 53
`
`
`
`Daca File D:\LIHSDATA\742203.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/17/2015 6:57:19 PM
`Iniection Dace
`408705
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\742199.5
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\629 40!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (742203.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`4
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Repor rc
`
`Sianal
`sorted Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilution
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rmin l
`rllAU•sl
`:;
`I
`----1-------l------l------- l----------l----··--- l---------------------
`l
`8.670 BP
`0 . 2665 4013.03003 100 . 0000 Bromfenac
`
`Tota l ~
`
`4013.03003
`
`Result~ obtained with enhanced integracor!
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 ll/17/2015 7:10: 10 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 28 of 53
`
`CONFIDENTIAL
`
`PROL0337675
`
`PAGE 28 OF 53
`
`
`
`Daca File D:\LIHSDATA\742204.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/17/2015 7:12:05 PM
`Iniection Dace
`408705
`Sample Name
`Aca. Operacor
`GT
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\742199.5
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\62940!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110,100 (742204.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`5
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorced Bv
`ll/16/2015 2:21:49 PM
`Cal ib. Daca Modified
`Mul ciplier
`l. 0000
`l. 0000
`Dilucion
`Use Multiplier & Dilucion Factor with ISTI>s
`
`Signal l: DAD! A, Sig=266,4 Ref=360,l00
`
`Peak RetTille TYPe Width
`Area
`Name
`Ar•~a
`rminl
`rminl
`rllAU•sl
`:;
`I
`----l-------1------l-------l----------l----··--- l---------------------
`l
`8.670 BP
`0 . 2667 4010.88867 100 . 0000 Bromfenac
`
`Tota l ~
`
`4010.88867
`
`Result~ obtained with enhanced integracor !
`1 Warnings or Errors :
`
`Warning : Invalid calibration curve, (Bromfo~nac)
`
`••• End of Report •••
`
`Instrument 1 ll/17/2015 7:24:56 PM GT
`
`Chromatographic Dataji-om the Stability Evaluation ofBromfenac Sodium Drug Product Samples for Potency, 1/1212016,
`page 29 of 53
`
`CONFIDENTIAL
`
`PROL0337676
`
`PAGE 29 OF 53
`
`
`
`Daca File D:\LIHSDATA\742205.0
`
`STI> A
`
`Sa.ple Name: 408705
`
`ll/17/2015 7:26:49 PM
`Iniection Dace
`408705
`Sample Name
`GT
`Aca. Operacor
`Inscrumenc 1
`Aca. Inscrumenc
`D:\LIMSDATA\742199.5
`Seauence File
`: C: \HPCHEM\ 1 \ME1l!ODS\62940!S02. M
`Method
`: ll/16/2015 3:25:25 PH bv I"T
`La~t chanaed
`I>AI>1 A. Sig•2ell.4 Rtfs3110.100 (742205.1>)
`
`Sea. Line
`Locacion
`Ini
`Inj Volwae
`
`6
`Vial 2
`1
`5 Ill
`
`mAU
`
`200
`
`150
`
`100
`
`Area Percenc Reporrc
`
`Sianal
`sorced Bv
`11/16!2015 2:21:49 PM
`Cal ib. Da
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