Quality Control Department

Q. C. # RM-22117

Raw Material Analysis

ONDANSETRON
HYDROCHLORIDE
 Quality Control Department

CERTIFICATE OF ANALYSIS

ONDANSETRON
HYDROCHLORIDE
(Raw Material)
Analysis Date: 23-04-2022 Doc. No: QC-017
Q.C. NO: RM-22117 MFG. DATE: 01-2022 EXP. DATE: 01-2025

BATCH NO: DXP-17-101 QUANTITY: 35.000 Kg No. of Containers: 02

SOURCE: Surge Laboratories (Pvt>) Limited, Karachi-Pakiatan.

QUALITY CONTROL ANALYSIS

TEST APPLIED SPECIFICATIONS (USP) RESULTS

Description White to off white colored enteric coated spherical pellets. Conform to Specs.

Identification Active Duloxetine (as HCl) should be +ve Conform to Specs.

Water Content (By NMT 5.0% 1.65%

KF)

Dissolution Test 1. 0.1N HCl, RPM 100, Temp. 370C, NMT 10% should 7.59%
release in 2 hours.
Test 2 (USP
Apparatus 2) 2. In Phosphate Buffer pH 6.8, NLT 80% should release 87.92%
in 60 min.

Assay (Duloxetine) on 17.00% (90 – 110 %) of the labeled claim) 18.30%

as is basis

Q.C. Remarks: Results complies with “USP” Specifications”. Raw material released for production use.

____________ _____________________
Q.C. Analyst Quality Control Manager
 Quality Control Department

STANDARD ANALYTICAL PROCEDURES

RAW MATERIAL: Duloxetine (as HCl) ECP SOP No: QC/RMA-09

17.00%
Issued On: 01-08-2018 Next Review: 01-08-2021 Control: d.qc.rm.sop.doc

SPECIFICATIONS: USP Specifications

DISSOLUTION: USP Test 2, Apparatus 2 (Paddle Apparatus)

1. Medium: 750 mL of 0.1N HCl, RPM: 100, Temp. 370C, Time: 2 hours
Limit: NMT 10% should release within 2 hours.

2. Medium: 1000 mL of Phosphate Buffer pH 6.8 (250 mL of 0.2M tribasic sodium phosphate
+ 750 mL of Acid medium used, set pH to 6.8 if required), RPM: 100, Temp. 37 0C, Time: 60
minutes
Limit: NLT 80% should release in 60 minutes.

Procedure: Acid Medium

Sample Preparation:
Add the pellets weight equivalent to 50 mg of Duloxetine (as HCl) in each 6 baskets of the
dissolution apparatus and fill each basket with 1000 ml of 0.1 N HCl. Rotate the peddles at 100
RPM. Take sample after 2 hours and get the absorbance at the peak maxima in the range of
200nm to 400nm.
The dilution of the final solution will be;
Duloxetine 50 mg per 1000 ml × 20 ml /50 ml ≡ 0.02 mg/ml of Duloxetine
Standard Preparation:
Take 50 mg of Duloxetine (as HCl) WS in 100 ml volumetric flask, dissolve in Methanol,
shake frequently and make the volume up to the mark with same solvent, take accurately 2 ml
of this solution into a 50 ml volumetric flask and make the volume up to the mark with 0.1N
HCl. Get absorbance at the peak maxima in the range of 200nm to 400nm (292 nm).
The dilution of the final solution will be;
Duloxetine 50 mg per 100 ml × 2 ml /50 ml ≡ 0.02 mg/ml of Duloxetine

Calculate the Assay for Duloxetine (as HCl) in sample solution using the following formula.

Abs Sp Wt Std 2 1000

----------- × --------- × ----- × --------- × Potency of working standard
Abs Std 100 100 Wt Sp.

= % age of Duloxetine (as HCl) released in 0.1N HCl after 2 hours.

Limit: NMT 10% should release
Procedure: Buffer Medium
Sample Preparation:
Add the pellets weight equivalent to 50 mg of Duloxetine (as HCl) in each 6 baskets of the
dissolution apparatus and fill each basket with 1000 ml of Phosphate buffer. Rotate the peddles
at 100 RPM. Take sample after 45 min and get the absorbance at the peak maxima in the range
of 200nm to 400nm.
The dilution of the final solution will be;
Duloxetine 50 mg per 1000 ml × 20 ml /50 ml ≡ 0.02 mg/ml of Duloxetine
Standard Preparation:
Take 50 mg of Duloxetine (as HCl) WS in 100 ml volumetric flask, dissolve in Methanol,
shake frequently and make the volume up to the mark with same solvent, take accurately 2 ml
of this solution into a 50 ml volumetric flask and make the volume up to the mark with 0.1N
HCl. Get absorbance at the peak maxima in the range of 200nm to 400nm (292 nm).
The dilution of the final solution will be;
Duloxetine 50 mg per 100 ml × 2 ml /50 ml ≡ 0.02 mg/ml of Duloxetine

Calculate the Assay for Duloxetine (as HCl) in sample solution using the following formula.

Abs Sp Wt Std 2 1000

----------- × --------- × ----- × --------- × Potency of working standard
Abs Std 100 100 Wt Sp.

= % age of Duloxetine (as HCl) released in Phosphate buffer pH 6.8 after 60 min.
Limit: NLT 80% should release
ASSAY:

Duloxetine (as HCl) ECP 17.65% (By UV-Visible Spectrophotometer)

Solvent:
Methanol

Sample Preparation:
Take the pellets weight equivalent to 50 mg of Duloxetine (as HCl) in a 100 ml volumetric flask,
dissolve the pellets in about 60 ml of Methanol solution by using the ultrasonic bath for 10-15
min at 500C. Make the volume up to the mark after cooling it at room temperature. Then take
accurately 2 ml of this solution in a 50 ml volumetric flask and make the volume up to the mark
with methanol. Get the absorbance at the peak maxima in the range of 200nm to 400nm.
The dilution of the final solution will be;
Duloxetine 50 mg per 100 ml × 1 ml / 50 ml ≡ 0.01 mg/ml of Duloxetine

Standard Preparation:
Take 50 mg of Duloxetine (as HCl) WS in 100 ml volumetric flask, dissolve in methanol, shake
frequently and make the volume up to the mark with same solvent, take accurately 2 ml of this
solution into a 50 ml volumetric flask and make the volume up to the mark with same solvent.
Get absorbance at the peak maxima in the range of 200nm to 400nm.

Calculate the Assay for Duloxetine (as HCl) in the sample using the following formula:

Abs Sp Wt Std 1 100 50

----------- × --------- × ---- × -------- × ----- × Potency of working standard
Abs Std 100 50 Wt Sp 1

= % age of Duloxetine (as HCl) as labeled claim.

Assay Limit: 90 – 110 % of the labeled claim.

____________ _____________________
Q.C. Analyst Quality Control Manager