SIDDHARTHA PHARMACEUTICALS Pvt. Ltd.

RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 1 of 7
Date GENERAL INFORMATION

Structure

Formula C14H11Cl2NO4

Mol. Wt. 328.2

Category Antiamoebic

Retest Period 12 months

Reference IP 2018

SPECIFICATION

S.N TESTS SPECIFICATION

1. Description A white or almost white, crystalline powder; odourless or almost odourless.

2. Solubility Freely soluble in chloroform; slightly soluble in ethanol (95%) and in ether;
very slightly soluble in water.

3. Identification A. IR
PREPARED BY CHECKED BY APPROVED BY
SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE
 SIDDHARTHA PHARMACEUTICALS Pvt. Ltd. RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 2 of 7
Date B. UV
C. A white precipitate is produced.
4. Free acidity Not more than 1.3 ml is required

5. Related substances Any secondary spot in the chromatogram obtained with the test solution is not
more intense than the spot in the chromatogram obtained with the reference
solution.

6. Sulphated ash Not more than 0.1%

7. Loss on drying Not more than 0.5%

8. Assay Diloxanide Furoate contains not less than 98.0% and not more than 102.0% of
C14H11Cl2NO4, calculated on the dried basis.

9. Storage Store protected from light.

METHOD OF ANALYSIS

S. N. Tests and procedure

1. Description:

Carefully weigh about 5.0 g of sample in a Petri dish, distribute the sample as evenly as practicable by
gentle sidewise shaking of the dish and check the appearance of sample which should be a white or
almost white, crystalline powder; odourless or almost odourless.

PREPARED BY CHECKED BY APPROVED BY

SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE
 SIDDHARTHA PHARMACEUTICALS Pvt. Ltd. RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 3 of 7
Date
2. Solubility:

Take a sample powder of about 1.0 g in a test tube or in a beaker, pour the suitable solvent, mix it and
check the solubility of sample as per directed in a monograph.

Freely soluble in chloroform; slightly soluble in ethanol (95 %) and in ether; very slightly soluble in
water.

Descriptive Terms Volume of solvent required for 1 g of solute

Freely soluble in chloroform From 1 to 10 for 1gm of solute

Slightly Soluble in ethanol (95 %) and in From 100 to 1000 for 1gm of solute
ether

Very Slightly Soluble in water From 1000 to 10,000 for 1gm of solute

3. Identification:

A. Determine by infrared absorption spectrophotometry. Compare the spectrum with that

obtained with diloxanide furoate WS or with the reference spectrum of diloxanide furoate.
B. When examined in the range 230 nm to 360 nm, a 0.001% w/v solution in ethanol (95 %)
shows an absorption maximum only at about 258 nm; absorbance at about 258 nm, about 0.7.
(25 mg in 50 ml and 1 ml to 50 ml)
C. On 20 mg determine by the oxygen-flask method, using 10 ml of 1 M sodium hydroxide as the
absorbing liquid. When the process is complete, acidify the liquid with nitric acid and add
silver nitrate solution; a white precipitate is produced.

PREPARED BY CHECKED BY APPROVED BY

SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE
 SIDDHARTHA PHARMACEUTICALS Pvt. Ltd. RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 4 of 7
Date
4 Free acidity:

Shake 3 g with 50 ml of water, filter and wash the residue with 3 quantities, each of 20 ml, of water.
Titrate the combined filtrate and washings with 0.1 M sodium hydroxide using phenolphthalein
solution as indicator; not more than 1.3 ml is required.

5. Related substances: Determine by thin-layer chromatography, coating the plate with silica gel
HF254.

Mobile Phase: A mixture of 96 volumes of dichloromethane and 4 volumes of methanol.

Test Solution: Dissolve 0.5 g of substances under examination in 5 ml of chloroform.

Reference solution: Dilute 1 ml of the test solution to 100 ml with chloroform and mix. Dilute 5 ml
of the resulting solution to 20 ml with chloroform.

Apply to the plate 5 µl of each solution. After development, dry the plate in air and examine in
ultraviolet light at 254 nm. Any secondary spot in the chromatogram obtained with the test solution is
not more intense than the spot in the chromatogram obtained with the reference solution.

6. Sulphated ash: Not more than 0.1 %.

Reagents Required:

1. Sulphuric acid
Procedure:

Heat a silica crucible or platinum crucible to redness for 10 minutes, allow to cool in a dessicator and

PREPARED BY CHECKED BY APPROVED BY

SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE
 SIDDHARTHA PHARMACEUTICALS Pvt. Ltd. RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 5 of 7
Date weigh. Put 1 g of substance under examination in the crucible and reweigh. Ignite the test gently at
first until the substance is thoroughly charred. Cool, moisten the residue with 1ml of Sulphuric acid,
heat gently until the white fumes are no longer evolved and ignite at 800˚ C ± 25˚ C until all black
particles have disappeared. Allow the crucible to cool, add a few drops of sulphuric acid and heat.
Ignite as before, allow to cool and weigh. Calculate the Sulphated ash using the following formula:
Repeat the operation until two successive weighing do not differ by more than 0.5mg.

Calculate the Sulphated ash using the following formula:

Sulphated ash in % w/w= ( c – a ) X 100

( b – a)
Where, a = wt. of empty crucible in g.

b = wt. of crucible & sample in g.

c = wt. of Crucible & residue in g.

7. Loss on Drying: Not more than 0.5 % determined on 1.0 g by drying in an oven at 105°.

Procedure:

Weigh a glass-stoppered, shallow weighing bottle that has been dried under the same conditions to be
employed in the determination for 30 minutes. Transfer about 1.0 g of sample to the bottle which is
specified in the individual monograph, cover it and accurately weigh the bottle and the contents.
Distribute the sample as evenly as practicable by gentle sidewise shaking to a depth not exceeding
10mm.
Dry the substance by placing the loaded bottle in the drying chamber/oven at 105˚ C ± 2˚ C for a
constant weight, remove the stopper and leave it also in the chamber. After drying is completed, open

PREPARED BY CHECKED BY APPROVED BY

SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE
 SIDDHARTHA PHARMACEUTICALS Pvt. Ltd. RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 6 of 7
Date the drying chamber/oven, close the bottle promptly and allow it to cool to room temperature in
desiccators before weighing. Weigh the bottle and the contents.
Calculate the Loss on Drying (LOD) using the following formula:

LOD in % w/w = (b – c) X 100 where, a = wt. of empty weighing bottle in g.

(b – a) b = wt. of weighing bottle & sample in g.
c = wt. of weighing bottle & dried sample in g

8. Assay :

Dissolve 0.3 g in 50 ml of anhydrous pyridine. Titrate with 0.1 M tetrabutylammonium hydroxide,

determining the end-point potentiometrically. Carry out a blank titration.

1 ml of 0.1 M tetrabutylammonium hydroxide is equivalent to 0.03282 g of C14H11Cl2NO4.

Standardization of 0.1 M tetrabutylammonium hydroxide

Weigh accurately about 0.4 g of benzoic acid, dissolve in 80 rnl of dimethylformamide, add a few
drops of a 1 per cent w/v solution of thymol blue in dimethylformamide and. Titrate with the
tetrabutylammonium hydroxide solution to a blue end-point. Protect the solution from atmospheric
carbon dioxide throughout the titration. Perform a blank determination and make any necessary
correction.

1 ml of 0.1 M tetrabutylammonium hydroxide is equivalent to 0.01221 of C7H6O2

9. Storage: Store protected from light.

Reference: IP 2018; Volume-II (Page No. 1840-1841)

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SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE
 SIDDHARTHA PHARMACEUTICALS Pvt. Ltd. RM Code: RA012
RMS No.: RAS012
Madhawaliya,Tilottama-15, Nepal
Supersede No.RAS012.05
RAW MATERIAL SPECIFICATION (ACTIVE)
Material Name:- DILOXANIDE FUROATE
Issue Date 25-02-2021 Effective Date
Next Revision 24-02-2026 Page Number 7 of 7
Date END OF SPECIFICATION

PREPARED BY CHECKED BY APPROVED BY

SIGNATURE
NAME SANGITA KC PASHUPATI YADAV BHOJ RAJ BASHYAL
DESIGNATION/ Sr. QC OFFICER/QC Sr. QC OFFICER/QC QA MANAGER/QA
DEPT.
DATE