MEEN
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`RVICES
`
`Project Code No. 16-35361
`
`CONFIDENTIAL REPORT
`
`Sterner, Kessler, Goldstein, Fox LLC
`
`Prepared By:
`Avomeen Analytical Services
`4840 Venture Dr.
`Ann Arbor, M/48108
`Issued Date: June 30, 2016
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
`Avomeen Analytica l Services I 4840 Venture Drive, Ann Arbor, M148108 Services I www.avomeen.com I800-930-S4SO
`Page 1 of 21
`
`PLAINTIFFS'
`TRIAL EXHIBIT
`PTX0129
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 739
`
`PTX0129-00001
`
`1
`
`CIP2028
`Argentum Pharmaceuticals LLC v. Cipla Ltd.
`IPR2017-00807
`
`

`

`MEEN
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`RVICES
`
`To :
`
`Josephine Kim
`Sterne, Kessler, Goldstein & Fox PLLC
`Phone: 202-7728896
`Email: joskim@skgf.com
`
`Project Code No. 16-35361
`
`Testing of Fluticasone and Azelastine Nasal Spray
`
`Thank you for contacting Avomeen Analytical Services for testing of Fluticasone and Azelastine Nasal
`Spray. Following are the results, methodology, and data associated with our analysis.
`
`Avomeen 10
`
`Table 1: Sample description
`Batch Number
`Sample Description
`
`Sample 1
`
`053116ST1395
`
`A16009SV
`
`Boxes of AZEFLO N/S drug product, LUPIN
`
`Expire Day
`
`01/2018
`
`Sample 2
`
`053116ST1396
`
`DND0214
`
`Boxes of NASOMAC -AF drug product, MACLEODS
`
`10/20/2017
`
`Sample 3
`
`053116ST1398
`
`MS1476
`
`Boxes of COMBINASE AQ drug product, CADI LA
`
`12/2017
`
`Sample 4
`
`053116ST1399
`
`ASA16002
`
`Boxes of FLORESP AZ Drug product, EMCURE
`
`01/2018
`
`Sample 5
`
`053116ST1400
`
`1601009
`
`Boxes of EZICAS AZ Drug Product, I NT AS
`
`12/2017
`
`Sample 6
`
`053116ST1401
`
`END0237
`
`Boxes of NASOCOM AZ drug product, DR REDDY
`
`11/2017
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`MEDA_APTX03504 7 40
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`PTX0129-00002
`
`2
`
`

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`MEEN
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`RVICES
`
`Project Code No. 16-35361
`
`Figure 1: Samples as received
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`MEDA_APTX03504 7 41
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`PTX0129-00003
`
`3
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`

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`MEEN
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`RVICES
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`Project Code No. 16-35361
`
`Executive Summary
`
`The testing results of Fluticasone and Azelastine Nasal Spray for particle size, pH Value, EDTA, Glycerin,
`Polysorbate 80, and MCC are shown in Table 2. The accuracy of each measurement will be within five
`relative percent per excipient. The information of APis and the preservatives on the label is also included
`in Table 3.
`
`Table 2: Testing resu lts for particle size, PH Value, EDTA, Glycerin, Polysorbate 80, and MCC
`Sample 1
`Sample 2
`Sample4
`Sample 5
`Sample 3
`
`Sample 6
`
`Ethylenediaminetetraacetic Acid (EDTA) (wt
`%)
`Glycerin (wt %)
`Polysorbate 80 (wt %)
`Micro Crystalline Cellulose with
`carboxymethyl cellulose (wt %)
`Particle Size Mean Diameter(nm) by ZetaPALS
`Particle Size Mean Diameter( 1-1m) by light
`microscopy
`pH Value
`
`<0.0001
`
`<0.0001
`
`0.02
`
`<0.0001
`
`<0.0001
`
`<0.0001
`
`2.1
`Detected
`
`2.4
`Detected
`
`2.0
`Detected
`
`3.0
`Detected
`
`2.4
`Detected
`
`2.5
`Detected
`
`2.8
`
`2.7
`
`2.9
`
`460.4
`
`309.8
`
`442.9
`
`2.9
`
`460.9
`
`2.9
`
`2.9
`
`452.2
`
`391.7
`
`1.14 ±0.32
`
`0.84±0.38
`
`0.98±0.40
`
`0.98±0.42
`
`1.02±0.41
`
`0.84±0.28
`
`6.21
`
`6.32
`
`5.75
`
`6.27
`
`6.33
`
`6.33
`
`Table 3: Information on the label for APis and preservatives
`Sample 1
`Sample 2
`Sample 3
`Sample 4
`
`Azelastine Hydrochloride IP (W/v)
`
`Fluticasone Propionate IP (W/v)
`Benzalkonium Chloride Solution IP (W/v)
`Phenylethyl AlcohoiiP (W/v)
`
`0.14
`
`0.05
`0.02
`0.25
`
`0.14
`
`0.05
`0.01
`0.25
`
`0.14
`
`0.05
`0.01
`0.25
`
`0.14
`
`0.05
`0.02
`0.25
`
`Sample 5
`
`Sample 6
`
`0.14
`
`0.05
`0.01
`0.25
`
`0.14
`
`0.05
`0.01
`0.25
`
`Quality Statement
`The work reported herein was conducted non- GMP and was not reviewed by Quality Assurance. All
`data in this report accurately reflects the raw data stored in the archives of Avomeen Analytical Services.
`
`Analytical Testing
`
`High Performance Liquid Chromatography (HPLC) Analysis for Ethylenediaminetetraacetic Acid (EDTA)
`Instrument: Agilent 1100
`Column: Supelco Uchrosphere RPC18, 250 mm x 4.6 mm, 5 J.lm
`Column Temperature: 3o•c
`Flow rate: 1 ml/min
`Injection Volume: 10 J.ll
`Mobile phase: 25 mM sodium acetate buffer with 1 mM tetrabutylammonium bromide in 950 ml
`deionized water and SO ml Methanol, pH 4.0, isocratic 20 min
`Detector wavelength: 265 nm
`
`EDTA standard preparation : EDTA standard was derivatized with a ferric chloride solution and analyzed
`by HPLC-UV. An EDTA standard (EDTA content 1.002 mg/mL) stock solution was prepared in D.l. water. 5
`ml of the EDTA standard solution was derivatized by 3 ml of ferric chloride solution (3.2 mg/ml) in 50
`ml volumetric flask. The mixture was shaken and kept in the oven at 7o•c for 20 min, and finally the
`
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`4
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`

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`MEEN
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`RVICES
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`Project Code No. 16-35361
`
`volume was made up with D. I. water. The derivatized EDTA solution was diluted and used for a
`calibration curve.
`Sample preparation: ~sao mg of samples was mixed with 5 ml of ferric chloride solution {3.2
`mg/ml) in 10 ml volumetric flask. The mixture was shaken well and kept in the oven at 70"C for 20 min,
`then cooled to room temperature, made with D.l. water and filtered for HPLC analysis. The amount of
`ferric chloride for standard and samples was assured to be in excess for the derivatization.
`
`High Performance Liquid Chromatography Analysis (HPLC-ELSD) for Polysorbate 80
`Apparatus : Agilent HPLC 1100 with Alltech 2000ES Evaporative Light Scattering detector (ELSD)
`Column: Kinetex, particle size 2.6 ~m, 150 x 4.6 mm, 100A
`ELSD conditions: Impactor On mode, 60"C drift tube temperature, 2.0 L/min nitrogen flow rate
`Injection volume : 10 ~L
`Column temperature : 30"C
`Column flow rate: 0.6 ml/min
`Run time : 50 min
`Mobile phase A: D.l. water with 0.1% Formic Acid
`Mobile phase B: Acetonitrile with 0.1% Formic Acid
`Gradient Elution:
`
`Time (min)
`
`Mobile Phase A (%)
`
`Mobile Phase B (%)
`
`0
`30
`45
`45.1
`so
`
`70
`0
`0
`70
`70
`
`30
`100
`100
`30
`30
`
`Sample preparation: about 1 g of each sample was dissolved individually with 5 ml of methanol and
`sonicated for 10 min at room temperature . After thoroughly mixing, the sample solution was filtered prior
`to injection into the HPLC-ELSD. 57 mg of Polysorbate 80 standard was dissolved in 25 ml methanol and
`diluted to 1000-3000 ~g/m Las calibration standards.
`
`HPLC-ELSD Analysis for Glycerin
`Instrument: Agilent 1100 equipped with Alltech 2000 evaporative light scattering detector (ELSD)
`Column: lmtakt Unison UK-Amino, 250 mm x 4.6 mm, 3 11m
`Column Temperature: 37"C
`Inject ion Volume: 20 Ill
`Mobile phase: A: D. I. water; B: Acetonitrile
`Gradient: !socratic 80% A, 20% B
`Run time : 30 min
`Flow rate : 1.0 ml/min
`ELSD parameters: Impactor ON mode
`Tube temperature : 42"C
`Gas flow rate : 1.5 L/min
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`MEDA_APTX03504 7 43
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`PTX0129-00005
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`5
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`

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`MEEN
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`RVICES
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`Project Code No. 16-35361
`
`Sample preparation : About 1 gram of sample was dissolved with 5 ml of methanol, sonicated for 10 min
`at room temperature. The sample solution was filtered prior to injection into the HPLC-ELSD. Glycerin
`standards in methanol in the range of 1000 to 6900 IJ.g/ml were prepared for calibration.
`
`Determination of Microcrystalline Cellulose with Small Amount of Carboxymethyl Cellulose
`The amount of microcrystalline cellulose was determined by loss of solvent washing and drying. Sample
`(around 600 mg) was accurately weighed in a tared Eppendorf tube, the tube was centrifuged at a speed
`of 14000 min·1 for 20 minutes. The supernatant was removed using a pipette and the residue was
`washed with D.l. water 1 ml, after the supernatant was removed, the residue was continued to be
`washed with methanol (2 x 1 mL) and D. l water (3 x 1 ml), the supernatant was removed and the
`residue was dried over nitrogen and weighed . The difference of tared empty Eppendorf tube and the
`residue with empty Eppendorf tube is the weight for microcrystalline cellulose. This method included
`small amount of carboxymethyl cellulose.
`
`Particle Size Distribution by using ZetaPALS:
`A small aliquot of the nasal spray samples were diluted individually in 5 ml of ultrapure water to form a
`slightly hazy solution. The sample was analyzed using a Zeta PALS particle size analyzer for the particle size
`distribution.
`
`Particle Size Distribution by using Light Microscope:
`A small aliquot of the nasal spray samples were analyzed by using Nikon TE2000 inverted microscope for
`particle size distribution.
`
`Determination of the pH Value of the Samples
`The pH value of samples was measured individually by the PH meter.
`
`Results
`
`Quantitation of Ethylenediaminetetraacetic Acid (EDTA)
`HPLC chromatogram of EDTA standard and calibration curve for EDTA standard are displayed in Figure 2.
`EDTA was found in sample 3 based on the match of retention time and HPLC chromatogram of sample 3
`was displayed in Figure 3. The weight percentage of EDTA in the sample 3 is listed in Table 2. EDTA in
`samples 1, 2, 4, 5, 6 are found below the limit of detection (1.5 ppm) and HPLC chromatogram of sample
`1, 2, 4, 5, 6 were displayed in Figure 3.
`
`Testing of Polysorbate 80 in the Samples
`Expanded HPLC chromatogram of polysorbate 80 standard was displayed in Figure 4. Polysorbate 80 was
`found in all of the samples based on the match of retention time and HPLC chromatogram of samples
`were displayed in Figure 5.
`
`Quantitation of Glycerin
`HPLC chromatogram of glycerin standard and calibration curve for glycerin standard are displayed in
`Figure 6. Glycerin was found in samples based on the match of retention time and HPLC chromatogram
`
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`MEDA_APTX03504 7 44
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`PTX0129-00006
`
`6
`
`

`

`MEEN
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`RVICES
`
`Project Code No. 16-35361
`
`of samples was displayed in Figure 7. The weight percentage of glycerin in the samples were listed in
`Table 2.
`
`Quantitation of Microcrystalline Cellulose with Small amount of Carboxymethyl Cellulose
`The amount of microcrystalline cellulose was determined by weight loss through solvent washing and
`drying. FTIR was used to characterize the microcrystalline cellulose in the sample. The FTIR spectrum for
`microcrystalline cellulose standard, samples and overlaid FTIR spectrum for the microcrystalline
`cellulose and samples were displayed in Figure 8. Sample 2 and sample 6 showed some trace of carbonyl
`group at -1700 cm·l, indicating presence of small amount of carboxymethyl cellulose.
`
`Particle Size Distribution by using ZetaPALS:
`Results for the particle size mean diameter (nm) of the samples is listed in the Table 2. The distribution
`data for each sample was displayed in Figure 9.
`
`Particle Size Distribution by using Light Microscope
`Results for the particle size mean diameter (11m) of the samples is listed in the Table 2. The distribution
`data and imagine for each sample were displayed in Figure 10.
`
`pH Value of the Samples
`Results for the particle size mean diameter (nm) of the samples is listed in the Table 2.
`
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`MEDA_APTX03504 7 45
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`PTX0129-00007
`
`7
`
`

`

`MEEN
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`RVICES
`
`Figures
`
`EDTA
`
`Project Code No. 16-35361
`
`••
`...
`
`..
`.. ··
`
`y = 14843x- 4.2778
`R1 = 1
`
`...
`. ··
`...
`
`...
`
`.. ······
`.. ·
`...
`
`...
`.. ··
`
`.. ······
`
`...
`...
`
`.-···· ~·· ~·.
`
`0.02
`
`0.06
`0.04
`Cone. mg/ml
`
`0.08
`
`0.1
`
`1400
`
`1200
`
`1000
`
`800
`
`600
`
`400
`
`200
`
`<!
`UJ cc
`<!
`
`0
`
`0
`
`70 ~
`eo ~
`!50 ~
`<II ~
`31l ~
`
`20 ~
`
`10 ~
`D~~~~~~~~~~~~~~~~ ~==~~~~~~~~~~~~~~~~~=,l
`~~~ 10
`.~ ,~~
`
`2
`
`4
`
`Cl
`
`\
`
`8
`
`10
`
`Figure 2: Calibration curve for EDTA standard (top) and HPLC chromatogram of EDTA standard (bottom)
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`MEDA_APTX03504 7 46
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`PTX0129-00008
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`8
`
`

`

`MEEN
`
`RVICES
`
`DA.D1 8 . Sl~S:5,.q R ~:Poff(mh sl:tm edt<~ 115--2· 18 '201&-00-02 11-37-46'1007-9-:umplt 1 0)
`
`Project Code No. 16-35361
`
`A: Sample 1
`
`..r-I.V>.
`
`..... ~
`
`I
`
`m.OI.J"
`0.4 -:
`
`0.2 0:: ~
`
`0
`
`.().2 :
`
`,...
`
`.().4 ~
`
`..(] .0-~~~~~
`e
`4
`2
`
`8
`
`.-~
`10
`12
`
`14
`
`HI
`
`18
`
`rrin
`
`DAD1 9 , Sig=26t5,4 Ref=off(mh stern adl a 6·2·16 2016-06-02 11-37-46'DOQ-10-sample 2.0 }
`
`m.'U :
`0.4 ~
`
`0.2 ~ ~
`
`0
`
`.().2 ~
`
`8: sample 2
`
`I'~~
`
`~
`
`I
`
`..0,4 ..:
`
`-4.(1 .
`
`m.'U :
`12 ~
`
`10 ~
`a-:
`
`2
`
`•
`
`0
`
`~~~
`8
`10
`
`12
`
`14
`
`10
`
`DAD1 B. Slo=2t!5 .4Rofaoff (mhs!tln odl•!l-2· 111 201!1-0e!-02 11·37·'11m11 ·11·um plo3.D)
`
`EDTA
`
`C: Sampl.,3
`
`--~,-.........----1
`
`18
`
`mn"l
`
`(1-:
`"-:
`2 ~
`o-:
`--~-~~~-~~~~~---~-~~---~---~---~-~~---
`e
`a
`rrin
`16
`2
`12
`14
`10
`18
`
`.
`
`~
`\
`
`DAD1 B, S l g=26~ARofaofl(mh s! o m odl i11·2· 10 20 10.0!!-0211·37-401025·:N·um plo4 D)
`
`m.'U
`
`0.2 ~
`
`0 .
`
`-11.2
`
`0 4 ~
`
`0 : Sample 4
`
`-,-
`
`~~
`
`.() .4
`
`-'Ill
`
`:
`
`..--.--~
`2
`4
`
`6
`
`8
`
`10
`
`~
`
`12
`
`14
`
`~~
`16
`18
`
`rrin
`
`DAD\ 8 , Sig--265 ,4 Ret-off (mhstem edt.. 0-2·10 20 10-00-02 11·37-'lf!'D27·31-sam ple O.D)
`
`Figure 3: HPLC chromatogram of sample l(A), sample 2(B), sample 3(C), sample 4(D), sample S(E) and
`sample 6(F)
`
`~--~~---.-~~~~
`10
`12
`
`14
`
`16
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`MEDA_APTX03504747
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`PTX0129-00009
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`9
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`

`

`MEEN
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`RVICES
`
`8
`
`6
`
`4
`
`2
`
`0
`
`Project Code No. 16-35361
`
`polysorbate 80
`
`v = 1.224x- 2.1~Qs··•
`R2 = ~:i9~1
`••
`
`0
`
`2
`
`4
`
`6
`
`8
`
`10
`
`ADC1 A ADC1 CHANNEL A(mh stern po~ M-16 2016-06·04 11-40·42'037·1l801.D)
`
`po~sorbate 80
`
`/
`
`J
`
`,-.,.-,..-,--rr-r-r--r-rr--r-~r~,....r~~r-r-r--r-r~~""""""'r-rr-r-~r-rr-r-,..-,--rr-r-~
`
`2\
`
`23
`
`24
`
`2
`
`8
`
`29
`
`I
`
`Figure 4: Calibration curve for polysorbate 80 standard (top) and expanded HPLC chromatogram of
`polysorbate 80 standard (bottom)
`
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`MEDA_APTX03504 7 48
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`PTX0129-0001 0
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`10
`
`

`

`MEEN
`
`RVICES
`
`ADC1 A. ADC1 CHANt1EL A(mh stem polyG-416 2016-00-0411-40-421046-1001 .0)
`
`~~ 55 "
`
`~2.5 ~
`~ ~
`47.6 ~F=~
`20
`
`I
`~
`22
`21
`
`Project Code No. 16-35361
`
`ADC1 A. AC'JC-1 CHAflPlELA(mh d.• m pol:fo-4- IC 201G-Oe·041t~7·1201 D)
`
`I
`
`L!J
`
`-
`
`"""' ~ &1
`)\JJ
`
`.,,, ~ ~.---;r;-..-~~;2--.-~23---r.----;;-~.--~.----;;-------a----a--~
`
`poly$0rbu te 80
`
`:
`50 .& .
`
`!Ill ; ••• .. .
`.... .. :
`
`ADC1 A.ADC1 CHANNEL A(m hstern polyG-410 201G-00·0411·45·42'D49·1<!01 D)
`
`rn'U :
`61 ~
`60 ~
`49 ~
`
`polysorbate 80
`
`48~L ~~=:::;:::;:::;::;:;:::~~=:=;=:::::;:==~~:.:::::::
`~
`....--r-,...-.....----r---~,...-1""'-"r--r-o-r..-~~r-..-r-r-..-,...--.---...-~_...,__,_,
`rrin
`20
`22
`23
`24
`25
`2G
`27
`28
`29
`
`21
`
`ADC1 AADC1 CHAN11ELA(mh.tern poly8-410 2016.00·0411·46·42'D49·1001 D)
`
`_.!J
`
`ADC1 A. ADC1 CAANNEL A (mh stern poly0-410 2018-00·0411-46-42050-1801 .0)
`
`:
`20
`
`;:x:
`
`r-
`~
`
`,----
`22
`
`,--~~-,------,-----,-----.-----,.---~-~·
`V
`23
`3
`2G
`28
`29
`~
`I
`
`ADC1 A. ADC1 CHANNELA(mh stern poly0·416 2016·06·0411-'lli·42'D51·2001 .D)
`
`~-L,..._,.~-:_···~ .. ~~.-5--~--;~
`~l~. ~~ 20
`
`2 1
`
`22
`
`23
`
`24
`
`25
`
`2G
`
`v
`
`28
`
`29
`
`Figure 5: Expanded HPLC chromatogram of Polysorbate 80 in samp le 1(A), sample 2(B), sample 3(C),
`sample 4(0), sample S(E) and sample 6(F)
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 11 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 7 49
`
`PTX0129-00011
`
`11
`
`

`

`MEEN
`
`RVICES
`
`Project Code No. 16-35361
`
`glycerin
`
`y = 3.1706x- 21.04
`...
`•.• -·······•
`R2 = 0.9985
`..•• ··• ··
`•·····
`·········
`... ....
`....
`
`.... -···
`
`8
`
`6
`
`4
`
`2
`
`0
`
`7
`
`7.5
`
`8
`L)
`
`85
`
`9
`
`ADC1 A. ADC1 CHANNeLA(mh st•rn glyoerin.6-3a·1B S 2016-ll6·03 11·44311\0nlineedlted..Q13 D)
`
`Figure 6: Calibration curve for glycerin sta ndard (top) and HPLC chromatogram of glycerin sta ndard
`(bottom)
`
`AOC 1 A. ADC1 CHAII NCL A(m hslern glycorln.6-3 a· 16 S 2016-Cie.Q311-44-31l\Onllne Edileci-.Q16.0)
`
`A: S<rmple 1
`
`AOC1 A. ACC 1 CHANN ELA (mh stern glyoorin.ll·3a-111 S 2018-Cl!l-0311·44-311\0ntone Edltod-0 17 D)
`
`~
`~~
`,:fr
`125 ~
`~,...?
`100 ~
`75~
`-......,_ .!\.
`50 ~ ,....._~r--~.--.-:::=::;:,-=:;=~~~=:;:.-=~====r==:;~=:;:~=~==r.-=:;:~=;:~=~=:;:,-=;:~=~=:;:~=;=,-=~=l
`a
`2
`4
`11
`10
`12
`14
`rrln
`
`glyc~erin
`
`0
`
`8 : Sample2
`
`......__
`
`ADC1 A. ADC1 CHANNELA(mh stem glyco rin.6·3a·16 S 201B·06·0311·44-39\0 nllneEdll od .. 018 .0)
`
`-
`
`150 .:
`
`too -:
`
`ADC1 A.AOC1 CHAIIIIELA(mhslorn gty04rin.6-3o·16 S 2016·06-00 11·44-311\0nllneEdrttd··0 1Q.O)
`
`1.,
`glyceri~ . ~""' .,,.,-t>
`-........}~
`
`0 : S<rmpl., 4
`
`50 -;l=====~=::: ~~ ~~.--~~~.--~ ~
`2
`4
`II
`8
`12
`10
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 12 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 750
`
`PTX0129-00012
`
`12
`
`

`

`MEEN
`
`RVICES
`
`ADC1 A.ADC1 CHAtHIE L A(mhsl•rn glyeorln.~·3•·1~ S 2016-06.0311·4439\0nllnoEdlled-020.0)
`
`Project Code No. 16-35361
`
`2
`
`0
`
`8
`
`10
`
`12
`
`ADC1 A, ADC I CHANNEL A (mhslorn glyoerln.e-3a-1e S 201~6-00 11-4430\0nllneEdlled··021.D)
`
`Figure 7: HPLC chromatogram of glycerin in the sample l(A), sample 2(B), samp le 3(C), samp le 4(D),
`sample S(E) and samp le 6(F)
`
`1-
`::§?.
`0
`
`A: Microcrystallin cellulose
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 13 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 751
`
`PTX0129-00013
`
`13
`
`

`

`MEEN
`
`RVICES
`
`C:Sample 2
`
`Project Code No. 16-35361
`
`3500
`
`3000
`
`2500
`
`cm-1
`
`2000
`
`600
`
`D: Sample 3
`
`45
`40
`3;~--------~----------~--------~--------~----------~--------~------~
`4000
`2500
`2000
`3500
`1500
`1000
`600
`3000
`cm-1
`
`E: Sample 4
`
`65
`~ooo~--------3~5o~o--------~3~oo~o--------~~~oo--------~2~ooo~--------,s~oo~------~,ooo~----~~o
`cm-1
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 14 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 752
`
`PTX0129-00014
`
`14
`
`

`

`MEEN
`
`RVICES
`
`Project Code No. 16-35361
`
`F: Sample 5
`
`6~----------~----------~----------~--------~----------~----------~------~
`4000
`1500
`1000
`3500
`3000
`2500
`2000
`600
`cm-1
`
`G:Sample 6
`
`3500
`
`3000
`
`2500
`
`~m -1
`
`2000
`
`H: overlaid FTIR Spectrum for MCC
`sUindard and samples
`
`N1me
`
`std
`> -
`> -S.mpleh
`> -
`s.mple2
`> -S.mple 3
`>
`S.mple4b
`> -
`SampleS
`"> -
`<;.mnl•fi
`
`DH<ription
`Sample 01S By Sample Slide Holder Dote W .. .
`Sample 018 By Sample Sl1de Holder Dote W .. .
`Sample 021 By Sample Slide Holder Date W ••
`Sample 017 By Sample Slide Holde• Dote W ..•
`Sample 020 By Sample Sl1de Holder Dole W .. .
`Sample 019 By Sample Slide Hold.,. Dote W .. .
`~mnlfl' 01.' Rv ~mnl,. Qirl,. Hnltf,._. n,..,. W._
`
`Figure 8: The FTIR spectrum fo r microcrystal cell ulose standard (A), sample l(B), sample 2(C), sample
`3(D), sample 4(E), sample S(F) sample 6(G) and overlaid FTIR spectrum for MCC standard and samples.
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 15 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 753
`
`PTX0129-00015
`
`15
`
`

`

`MEEN
`
`RVICES
`
`Project Code No. 16-35361
`
`MSDSummary
`
`Sample 1
`
`~D s 1 (tont>ned)
`Doe- Tine
`Jun 2. 2016 09"17:30
`Operolor I) a tim
`Elapsed Tmo OO·OS:OO
`Mean O..m.
`460.4 nm
`Rel Var
`0.087
`Skew
`19657
`
`7>
`
`...
`~ ~
`,
`•
`~·
`
`:
`_,....,
`
`'"'""
`
`3
`INcmbet
`1:0111' lor SJMeadthee! I
`Copy to Clpboa,-d I
`I
`
`Close
`
`I
`
`l:l[IJ
`.
`-
`
`,.
`
`~·
`
`.
`.
`.
`.
`....,.
`
`3
`INcmbet
`CopJO for S JMeadsheel I
`Copy to Cli¢oald I
`I
`I
`
`Close
`
`d{nm) G(d) C(d.
`2611
`0
`0
`2894
`0
`0
`320.1
`0
`0
`353.9
`0
`0
`3914 16
`7
`55
`432.8 100
`478.6 81
`93
`98
`529.3
`10
`565.3
`3 100
`647 2
`0 100
`715 7
`0 100
`
`d(nm) G(d) C(d
`791 4
`0 100
`875~ 0 100
`0 100
`9678
`0 100
`10702
`11835
`0 100
`1308 7
`0 100
`1447 2
`0 100
`1600.3
`0 100
`17697
`0 100
`19570
`0 100
`21641
`0 100
`
`d(nml G{d) C{d)
`2393. 1
`0 100
`26463
`0 100
`29264
`0 100
`3236.0
`0 100
`0 100
`3578.5
`39572
`0 100
`4375 9
`0 100
`4839.0
`0 100
`53511
`0 100
`5917 4
`0 100
`6543.6
`0 100
`
`s2 (Combioed)
`SallllleD
`Oole- me
`Jun 2, 2016 09"31 22
`Operalor D
`adtTWI
`Elapsed Tine 00 05.00
`Mean O..m.
`309.8nm
`ReL Vor.
`0358
`2_544
`Stew
`
`Sample 2
`
`d(nm) G(d) C(<f
`643
`0
`0
`96.5
`0
`0
`110.5 100
`41
`41
`0
`126.5
`0
`14.4.8
`41
`0
`165 8
`41
`41
`189.8
`0
`41
`217.2
`0
`41
`248 7
`0
`41
`28-0.7
`0
`41
`325.9
`0
`
`d(nm) G(d) C(d )
`d(nm) G(d) C(d
`·uo
`1651.5
`373 I
`l3
`0
`46
`81
`1890.6
`0 100
`427 I 83
`98
`2164 4
`0 100
`489.0
`41
`99 z•n.s
`0 100
`4
`559.8
`64!1.9
`1 100
`2836.5
`0 100
`3247.3
`100
`7337
`0 100
`0
`0
`0 100
`8399
`tOO
`3711.5
`961 .5
`0 100
`0 100
`•255.8
`1100 7
`0 100
`4872.0
`100
`0
`ssn.s
`1260. 1
`0 100
`0 100
`6385.1
`1442.6
`100
`0
`0 100
`
`MSD Summary
`
`Sample3
`
`SalllllaD
`s3 (tont>oned)
`Jun 2. 2016 10 42.00
`Dale- Tine
`O~lorD OdtTWI
`Elapsed Tme oo o5·oo
`Mean D~am. 442.9 nm
`Rel Var
`0.038
`Skew
`21989
`
`d[nm) G(d l C(d.
`254.4
`0
`0
`2n.9
`0
`0
`308.0
`0
`0
`338.8
`0
`0
`6
`372 .7
`9
`410 1 35
`29
`94
`451.1 100
`9 100
`496.3
`546.0
`0 100
`600.7
`0 100
`660.9
`0 100
`
`d(nm) G(dl C(d)
`d(nm) G{dl C(d
`n1.1
`0 100 2on6
`0 100
`'100
`799.9
`2285.6
`0 100
`0
`0 100
`25146
`880.0
`0 100
`0 100
`968.1
`2766.4
`0 100
`0 100
`3043.5
`1065.1
`0
`tOO
`0 100
`t171 .7
`3346.3
`0 100
`3683.6
`0 100
`1289.1
`0
`tOO
`'100
`1418.2
`40526
`0 100
`0
`4.458t
`1560.2
`0 100
`0 100
`1716.S
`0 100
`490S 0
`0
`tOO
`1888.t
`0 100
`0 100
`5396.2
`
`ll[[J
`.
`
`%
`
`"
`
`~·
`
`•
`
`.
`.
`__, ... ,
`
`•
`
`.
`.
`
`!000:1 0
`
`!Number
`
`3
`1:0111' for SJMead•heell
`I:OII!'lo~d I
`I
`I
`
`Close
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 16 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 754
`
`PTX0129-00016
`
`16
`
`

`

`MEEN
`
`RVICES
`
`MSOSummary
`
`Sample 4
`
`s,4 (Combiled)
`S..rrplell
`Jun 2, 2016 10 13' 16
`lm!e- Tmo
`Ope,..torll Odmrl
`Elopsed nne oo·o5:oo
`!.lean Olam.
`400.9 nm
`Rel Var
`0.032
`Skew
`24222
`
`Project Code No. 16-35361
`
`_,
`lill
`
`j
`•
`
`•
`
`i
`
`•
`
`•
`
`~·
`
`J..
`
`:0
`
`0
`
`!llO
`
`d(nm) G(d) C(d
`291.5
`0
`0
`317.4
`0
`0
`3456
`0
`0
`3764
`0
`0
`409.8
`14
`8
`4462 100
`70
`94
`465.9 40
`529.1
`8
`99
`5761
`2 100
`627 3
`0 100
`6830
`0 100
`
`d(nm) G(d) C(d)
`d(nm) G(d) C(d
`1897.6
`0 100
`7438
`0 100
`2066.3
`0 100
`8099
`0 100
`2249,9
`0 100
`8818
`0 100
`0 100 2«9.9
`9602
`0 100
`1045.6
`26676
`0 100
`0 100
`0 100
`0 100
`11385
`2904.7
`1239.7
`3162.9
`0 100
`0 100
`1349.9
`0 100
`3444.0
`0 100
`14698
`3750.1
`0 100
`0 100
`0 100
`1600.5
`4083.4
`0 100
`1742.7
`0 100
`«-<6.4
`0 100
`
`I Number
`:!]
`Copy for SP<eadd1eel I
`Copy to Clipbo111d I
`I
`I
`
`Close
`
`~~1m
`.
`,.
`...
`
`:
`
`:
`
`.
`.
`.
`.
`"""'
`.-
`
`!0
`
`-
`
`jN!.IIi>er
`
`:::J
`Copy 1 .. SP<eadohee( I
`Copy to Clipboold I
`I
`
`I
`
`Cto.e
`
`l!llJJ
`.
`- ...
`
`:
`
`:
`
`.
`.
`.
`.
`...,,
`
`Sri)
`
`,.
`.,.
`
`MSO Summary
`
`SampleS
`
`......
`
`Sa~O sS (Corrmed)
`Date-Tme
`Jun 2, 20 16 10.2•:0•
`Or>erator 0
`Eio!>'ed Trne oo o5·oo
`~lean Olrlm.
`452.2 nm
`Rei Vu
`0.219
`S<aw
`5152
`
`d(nm) Gld) C(d
`0
`0 1
`0
`0 I
`0
`0
`0.2
`0
`0
`03
`0
`0
`o.•
`0
`0
`06
`0
`0
`0
`0.9
`0
`1.2
`0
`0
`\8
`0
`0
`2.5 D
`0
`37
`0
`0
`
`d(nm) G(d) C(d
`d(nm) G(d ) C(d
`5.2
`273.8 37
`0
`0
`20
`75
`7.5
`392.4 100
`0
`0
`562.3 24
`88
`10.7
`0
`0
`805.8 19
`98
`0
`0
`154
`99
`1\54 8
`2
`221
`0
`0
`3\6
`1654 8
`1
`tOO
`0
`0
`•5.3
`0 237t.
`0
`0
`tOO
`3398.2 D 100
`64 .9
`0
`0
`93.1
`0
`4869.7
`tOO
`0
`0
`6918.3
`1334
`0
`0
`0 100
`1911
`0
`0 100000
`0 100
`
`MSD Summary
`
`Sample6
`
`Saqllell
`O.te-T"""
`
`s6 (Comllr1ed)
`Jun 2. 2016 10 33.20
`
`Opentor II ·-
`
`Eloi>'ed Trne 00 05:00
`lrr.!ean Otam
`391 7nm
`Rei. Var
`0 112
`H77
`Sl.ew
`
`,.
`,.
`,.
`
`d(nm) G(d) C(d
`105.6
`0
`0
`1218
`0
`0
`1404 22 H
`161 a
`0
`1865
`0
`215,0
`0
`247.9
`0
`I
`2858
`8
`329•
`379.8 20
`•37.8 100
`
`14
`15
`19
`31
`93
`
`d!nml G(d) C(d
`10 100
`504.7
`5819
`1 100
`6708
`0 100
`773 3
`0 100
`8914
`0 100
`•911.
`10277
`0 100
`56619
`0 100
`1164 7
`6527 t
`1365.8
`0 100
`752• 6
`0
`tOO
`157•5
`867<.4
`18151
`0 100
`0 100 10000 0
`2092.•
`
`d(nml G(d) C(d
`2412.2
`0 100
`2780.8
`0 100
`0 100
`32057
`36956
`0
`tOO
`•260.
`tOO
`0
`0 100
`tOO
`0
`0 100
`0
`tOO
`0 100
`0
`tOO
`
`:::J
`I'l!lllbeo
`Copy ... Spoeadsheet I
`Copy to Clilbollod I
`I
`
`Clcne
`
`I
`
`Figure 9: Zeta PALS particle size distribution of sample 1, sample 2, sample 3, sample 4, sample 5 and
`sample 6
`
`FDA Registered I cGMP Compliant Focilitv IDEA Licensed
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`Page 17 of 21
`
`HIGHLY CONFIDENTIAL-
`SUBJECT TO STIPULATED PROTECTIVE ORDER
`
`MEDA_APTX03504 755
`
`PTX0129-00017
`
`17
`
`

`

`MEEN
`
`RVICES
`
`•
`
`•
`
`Sample 1
`
`•
`
`•
`
`5um
`
`'"""""'
`I
`2
`a
`'
`•
`•
`..
`
`5
`
`7
`
`9
`10
`11
`12
`13
`
`15
`16
`17
`18
`19
`20
`21
`22
`23
`
`• ,,
`
`25
`26
`27
`28
`29
`30
`Mean !Jiml
`Sld(!.m)
`
`10
`11
`12
`
`"
`
`14
`15
`16
`17
`18
`19
`20
`21
`22
`23
`24
`25
`26
`27
`28
`29
`30
`... ..,(lim)
`Sld(,m)
`
`lpartlde
`1
`2
`3
`
`Project Code No. 16-35361
`
`d {um)
`0.665
`0.7:2,
`0.?21
`o.eoe
`D.I!IOS
`0.1322
`0.869
`0.869
`09'
`0.96B
`o.ese
`0.981
`0.981
`102
`1.0!2
`1,129
`1.129
`1.129
`1.129
`1.174
`1.29
`129
`1.3
`1.643
`1.452
`1522
`1.1597
`1.645
`1.66,
`1,S49
`11<
`o.n
`
`d (um)
`0 ,326
`0.469
`0.-'89
`MM
`0.469
`0.469
`0.516
`0.547
`0.588
`0588
`0.692
`0.692
`0.729
`0.734
`0.73.4
`o.nJ
`O.B15
`0.815
`0 .631
`o.e?a
`0.97!
`0.978
`0.978
`0.992
`1,008
`1.031
`1.317
`1.547
`1.?12
`1.972
`0.84
`0.38
`
`d(um)
`0.5
`0.5
`0.5
`0.5
`0.5
`0.75
`0.75
`0.75
`0.75
`0.75
`0.75
`0,75
`0.75
`0.791
`0,791
`0.79 1
`O.to1
`I
`I
`I
`1.031
`1.25
`1.25
`•.• 58
`1.<158
`1,5
`1.521
`1.381
`\ .677
`t.9!3
`0,94
`0.40
`
`10
`11
`12
`13
`14
`15
`16
`17
`II
`19
`20
`21
`22
`23
`
`"
`
`25
`26
`27
`28
`29
`30
`Mean(~ m}
`Std (!om)
`
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`

`

`MEEN
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`Project Code No. 16-35361
`
`d(um)
`0.17
`
`... ,.
`
`0682
`0.682
`
`. ....,
`
`I~J.al'tidll
`
`•
`
`6
`1
`•
`•
`to
`11
`12
`1:)
`1.11
`15
`1&
`17
`18
`18
`:zo
`:u
`22'
`23
`24
`2S
`21!o
`27
`28
`29
`30
`M«<M(IInl)
`Sld~m)
`
`0.68-2
`0.682
`0.703
`0.703
`o.n3
`0762
`0.7&2
`o.w
`0.169
`0.869
`O.WJ
`OOUI
`0..9UI
`09111!1
`o.sne
`~ .Gl7
`1.078
`1.193
`1. 193
`I,..
`l .$6.1.
`I 5U
`1.33a
`Ut-43
`2.053
`0.98
`0.42
`
`rlpalticJe
`I
`2
`3
`4
`.&
`6
`7
`a
`i
`10
`11
`12
`13
`14
`1s
`10
`11
`18
`19
`20
`21
`22
`~
`'24
`25
`26
`<7
`28
`2'il
`JO
`·~~M(Jil'l'l)
`S1d(j.jm'
`
`d(um)
`0.&
`0.527
`OSS9
`0559
`0&01
`0661
`D.l$67
`o.&a7
`0707
`0.707
`0?.45
`o.e»
`o.m
`ow
`o.e33
`I
`I
`10!'»4
`, 0$1
`, 118
`1.179
`1 344
`13-46
`1,414
`14s.&
`1,572
`1.Pi72
`tf171
`1.7 ..
`1 . 9~
`I 02
`o.•t
`
`~ panu:Je
`I
`2
`3
`
`10
`11
`12
`13
`14
`15
`16
`17
`us
`19
`20
`21
`22
`23
`24
`25
`20
`27
`2a
`29
`30
`Mean (lll'lJ
`Std (um)
`
`d (um)
`O.l33
`0.333
`0.5
`0.527
`0.601
`0.667
`0.667
`0.661
`0.667
`0.687
`0.687
`0.687
`0.745
`0.745
`0.833
`0.833
`0.8.5
`0.85
`0.65
`0.898
`O.!W3
`0.912
`1.05ol
`1.05-1
`U67
`1,167
`1.167
`1179
`1.179
`1.65
`0.84
`0.28
`
`Figure 10: The distribution data and representative imagine of sample 1, sample 2, sample 3, sample 4,
`sample 5 and sample 6
`
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`MEEN
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`RVICES
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`Project Code No. 16-35361
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`Description of Instrumentation Used
`
`Gas Chromatograph (GC): GC analysis is commonly used to separate and analyze vaporized volatile
`compounds. This system uses an inert gas to carry the sample through a separatory column, and then
`detects the retention time of different compounds in the column . Avomeen's scientists often use gas
`chromatography to help in the identification of an unknown compound, or mixture of compounds.
`Avomeen' s Gas Chromatography capabilities include autosampling, pyrolysis, flame ionization detection,
`thermal conductivity detection, and the use of a range of polar and non-polar columns.
`
`Reverse Phase High Performance Liquid Chromatography (rpHPLC): Avomeen uses Agilent 1100 series
`instruments with quaternary pumps. Detection modules include Refractive Index, Evaporative Light
`Scattering, UV variable wavelength and UV Diode Array Detectors. The quaternary pumps allow the use
`of variable solvent chemistry to optimize resolution and run time. Diode Array detection allows for
`collection of data from multiple wavelengths simultaneously. The system is optimized for reverse phase
`chromatography, which allows the analyst to utilize a highly polar mobile phase solution that carries the
`compound of interest though the chromatography column. The column contains a non-polar stationary
`phase that interacts w ith the compound of interest as it is pumped through the column. The compound
`eventually is released from the column and travels to the detector where a signal arises based on the
`compound's characteristic absorbance and retention time. The analog signal is converted to a usable
`chromatogram where the information about the compound can be analyzed with high accuracy and
`precision.
`
`Dynamic Light Scattering (DLS): DLS is a photometric technique for determining the size distribution of
`suspended particles in a liquid medium. The instrument reads the scattering pattern of light created by
`Brownian motion of suspended particles and calculates the corresponding size distribution. Results can
`be reported in terms of volume, intensity or number with volume being the primary reporting method
`for pharmaceutical work. If additional characteristics of the particles are known, the approximate weight
`of the particles can also be calculated.
`
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`MEDA_APTX03504 758
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`PTX0129-00020
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`
`

`

`MEEN
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`RVICES
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`Wrap Up
`
`Project Code No. 16-35361
`
`Testing results relate only to items tested. Test report shall not be reproduced, except in full, without
`approval from Avomeen, LLC in writing.
`
`Thank you for consulting with Avomeen Analytical Services. I