CERTIFICATE OF ANALYSIS

(Certificate No.: SPC240807 - 033 / V.02 )

Analysis Date : 05/08/2024 Re-test Date: 04/08/2027

Product Name : OLOPATADINE CARBALDEHYDE HYDROCHLORIDE
Chemical Name : (Z)-11-(3-(dimethylamino)propylidene)-6,11-dihydrodibenzo[b,e]oxepine-2-carbaldehyde
hydrochloride
Synonyms : NA
CAT No. : O030012
Batch Number : SP-0724-085
CAS No. : 2519517-78-1
Molecular Formula : C₂₀H₂₁NO₂.HCl
Molecular Weight : 343.85 g/mol ; 307.39g/mol (As base)
Storage Condition : Store at -20°C

Shipping Condition : Ice Shipment

ANALYTICAL INFORMATION:

Sr No TESTS RESULTS
1 DESCRIPTION Pale Yellow Solid

2 SOLUBILITY Soluble in DMSO and Methanol

3 IDENTIFICATION
1. 1H-NMR Conforms to the structure
2. MASS Conforms to the structure
3. IR Conforms to the structure
4 CHROMATOGRAPHIC PURITY (By HPLC, area 94.27%
Normalization)
5 TGA 1.95 %w/w
Weight Loss: (30°C to 105°C)(30° to 450°, rate: 20°C/min)
6 DEFINED POTENCY 92.43 %w/w
(By Mass Balance Method) [(100-TGA) x HPLC Purity /100]
Not for Human or Animal Consumption. Only for Analytical Testing Purpose

Prepared By : Neha G Gupta Approved By : Sneha Bhopi

(Sign & Date) 25/07/2024 (Sign & Date) 25/07/2024

Quality Accreditations: ISO 9001:2015, ISO 17034:2016, ISO/IEC 17025:2017, GLP Certified, DSIR

Simson Pharma Limited :Office :B-307, Sarita Building, Prabhat Indl. Estate. Nr. Dahisar Toll Naka, Dahisar (East), Mumbai - 400068.
Simson Life Sciences Pvt.Ltd :Shed No.6A, Type III, TSIIC, Prashanthi Nagar, Kukatpally, Hyderabad, Telangana-500072

Page 1 of 1
NMR Study: The NMR experiments were performed in 400 MHZ Bruker FT-NMR Spectrometer using
DMSO Solvent .1HNMR Chemical shifts are reported on the  scale in ppm in relative to TMS. The
assignment of protons is given below

Chemical ‘J’
No. of
S.No. Shift Multiplicity coupling Assignment of proton(s)
protons
, ppm constant
1. 2.66-2.83 M 8H - 8
2. 3.26-3.31 M 2H - 2
3. 5.01-5.52 M 2H - 2
4. 5.71-5.75 T 1H - 1
5. 6.99-7.01 D 1H - 1
6. 7.31-7.48 M 4H - 4
7. 7.71-7.74 T 2H - 2
8. 9.90 S 1H - 1
9. 10.25 S 1H - 1
Total No. of protons 22
Confirms to the structure
Remark :-

Note: The assignments are based on chemical shifts and multiplicities

Mass Spectral Data: The mass spectroscopy studies were performed on API 2000 mass spectrometer triple
quadrupole.
The mass spectrum in positive mode displayed a protonated molecular ion at m/z 308.1 corresponding to
[M+H]+ confirms the monoisotopic mass as m/z corresponding to the Molecular formula C20H21NO2
Solvent: methanol

S. No Composition Exact Mass Molecular Weight m/z value

1. C20H21NO2 307.16 307.39 308.1 (+ve mode)

Remarks:
1. Mass Peak at m/z 308.1 corresponds to base mass peak.
IR Study: The FTIR spectrum was recorded in the solid-state KBr pellet using Bruker spectrophotometer.
The IR data is tabulated below.

S.No Type of bond Specific type of bond Absorption peak cm-1

1. C=O Stretching 1680.41

2. C-N Stretching 1231.74

3. C-O Stretching 1104.98

 SAMPLE INFORMATI ON
Sample Name: SP-0724-085 Unknown Acquired By: System
Sample Type: 16 Sample Set Name: 20042024
Vial: 1 Acq. Method Set: Genral_method 08
Injection #: 10.00 ul Processing Method: LC PQ1
Injection Volume: 40.0 Minutes Channel Name: 254.0nm
Run Time: Proc. Chnl. Descr.: PDA 254.0 nm

Date Acquired: 05/08/2024 3:44:58 PM IST

Date Processed: 05/08/2024 4:27:53 PM IST

1.00

Peak3 - 20.478
0.90

0.80

0.70

0.60
AU

0.50

0.40

0.30

Peak8 - 26.928
.55279

Peak5 - 21.243

Peak6 - 23.093

Peak7 - 25.987
4 0 78
PPeeaakk21--1199.8

0.20

0.10

0.00

0.00 5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00

Minutes

Peak Name RT Area % Area

1 Peak1 19.529 185442 1.96
2 Peak2 19.857 8188 0.09
3 Peak3 20.478 8910868 94.27
4 Peak4 20.783 44949 0.48
5 Peak5 21.243 47707 0.50
6 Peak6 23.093 32202 0.34
7 Peak7 25.987 25103 0.27
8 Peak8 26.928 197978 2.09

User Name:SYSTEM Project Name: AUGUST-2024

Report Method: Default Individual Report_09 Date Printed:
Report Method ID: 1245 05/08/2024
Page: 1 of 1 5:06:44 PM
 Filename: ...Hydrochloride B. NO. SP-0724-085.tg8d
Operator ID: Roshan Kore
Sample ID: Olopatadine Carbaldehyde Hydrochloride B. NO. SP-0724-085
Sample Weight: 1.567 mg
Comment: SPL/00369/24-24
110
100
SIMSON ANALYTICAL LABORATORIES
90 Delta Y = 1.953 %
Volatile compound (LOD) at 105°C = 1.953%
80
70
60
Weight % (%)

50
40
30
20
10
0
-10
29 100 200 300 400 500 600 700 800 900
Temperature (°C)
7/24/2024 10:42:55 AM
1) Hold for 1.0 min at 30.00°C 4) Heat from 150.00°C to 900.00°C at 40.00°C/min
2) Heat from 30.00°C to 105.00°C at 20.00°C/min 5) Hold for 2.0 min at 900.00°C
3) Heat from 105.00°C to 150.00°C at 40.00°C/min