Oxytetracycline Dyhydrate RMA016

GENTRY PHARMACEUTICALS LTD.
Vangnahati, Sreepur, Gazipur.
QUALITY ASSURANCE DEPARTMENT

STANDARD TEST PROCEDURE OF RAW MATERIAL-ACTIVE INGREDIENT
Name of Material OXYTETRACYCLINE DIHYDRATE BP
Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01
Issue Date 01.07.2018 Effective Date: 10.07. 2018 Review Date: 10.07. 2021
Prepared by Checked by Approved by
Sign. & Date
Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin
Designation Sr. Quality Assurance Officer Quality Control Manager Quality Assurance Manager
CONTENT
1. Appearance
2. Solubility
3. Identification
4. PH
5. Water
6. Residue On Ignition
7. Assay
8. Revision History
ATTACHMENTS
1. Specification [SPEC/RMA016]
2. Specimen COA
DISTRIBUTION LIST
Section No. of Copy Received By (Signature & Date)
QC Laboratory 01
Page 1 of 6
WITHOUT PERMISSION FROM HEAD OF QUALITY ASSURANCE OR HIS/HER
DELEGATE, COPY OF THIS DOCUMENT IS STRICTLY PROHIBITED

Sign. & Date
Sl. No. Test Parameter Procedure BP
01. Appearance Yellow, crystalline powder.
02. Solubility Very slightly soluble in water. It dissolves in dilute acid and alkaline solutions
B. To about 2 mg add 5 mL of sulfuric acid R. A deep red colour develops.

Add the solution to 2.5 mL of water R. The colour becomes yellow.
C. Dissolve about 10 mg in a mixture of 1 mL of dilute nitric acid R and 5 mL

03. Identification
of water R. Shake and add 1 mL of silver nitrate solution R2. Any
opalescence in the solution is not more intense than that in a mixture of 1
mL of dilute nitric acid R, 5 mL of a 0.021 g/L solution of potassium chloride
R and 1 mL of silver nitrate solution R2.
4.5 to 7.5.
04 PH
Suspend 0.1 g in 10 ml of carbon dioxide-free water R.
05. Water 6.0 per cent to 9.0 per cent, determined on 0.250 g.
Page 2 of 6

Sign. & Date
06. Assay 95.0 per cent to 102.0 per cent (Anhydrous Substance).
A. ASSAY : BY HPLC
PROCEDURE :
1.Tetrabutylammonium hydrogen sulphate solution :

Dissolve 1 gm of tetrabutylammonium hydrogen sulphate in 100 ml of water.
Ad just with 1 M sodium hydroxide to PH of 7.5.
2. Edetate disodium solution :
Dissolve 0.04 gm of edetate disodium in 100 ml of water. Ad just with 1 M

sodium hydroxide to PH of 7.5.
3. Phosphate buffer PH 7.5

Prepare a mixture of 0.33 M dibasic potassium phosphate and 0.33 M mono
basic sodium phosphate (85: 15).
Adjust if necessary, by adding more of the appropriate component to a P H of
7.5.
4. Mobile Phase :
Transfer 200 ml of water, 50 gm of tertiary butyl alcohol to a 1000 ml of
Volumetric flask. Add 60 ml of Phosphate buffer P H 7.5, 50 ml of
tetrabutylammonium hydrogen sulphate solution, and 10 ml of edetate
solution dilute with water to volume.
5. Std. Soln. : Dissolve 20 mg of Oxytetracycline WS in 0.1 M hydrochloric
acid. Dilute to 25 ml with the same solvent.
6. Spl. Soln. : Dissolve 20 mg of Oxytetracycline in 0.1 M hydrochloric acid.
Dilute to 25 ml with the same solvent.
Page 3 of 6

Sign. & Date
07. CHROMATOGRAPHIC SYSTEM :

a. Column : 4.6 mm x 250 mm, Packing L21
b. Detective Wavelength : 254 nm
c. Flow rate : 1 ml/min
d. Injection volume : 20 ml
e. RSD : NMT 1.0%
08. Separately inject equal volumes of Std. Soln. and. Spl. Soln. into
Chromatograph, record the chromatograms and measure the peak responses
for the major peaks. Calculate the content by the formula:
Pu Ws P
% Content of Oxytetracycline = × ×F× ×100
Ps Wu 100
Here,
Pu = Peak area of the sample.

Ps = peak area of the standard.
Ws = Weight of the standard
Wu = Weight of the sample
F = Dilution factor
P = Potency of standard in percentage.
C. ASSAY: BY SPECTROPHOTOMETRY METHOD:

PROCEDURE :
Page 4 of 6

Sign. & Date
01. Std. Soln. : Dissolve 100 mg of Oxytetracycline Dihydrate WS in 60

ml of 0.1 M hydrochloric Acid and dilute to 100 ml with the same solvent.
Dilute 2 ml of the resulting solution to 100 ml with 0.1 M hydrochloric Acid.
02. Spl Soln. : Dissolve 100 mg of Oxytetracycline Dihydrate in 60 ml of

0.1 M hydrochloric Acid and dilute to 100 ml with the same solvent. Dilute 2
ml of the resulting solution to 100 ml with 0.1 M hydrochloric Acid.
3. Measure the absorbance of the Std. Soln. and. Spl. Soln. at 268 nm
against blank and calculate the content by the formula:
% Content of Oxytetracycline Dihydrate
Au Ws P
= ------ × ------ × F × ------- × 100
As Wu 100
Here,
Au = Absorbance of the Sample

AS = Absorbance of the Standard
Wu = Weight of the Sample
Ws = Weight of the Standard.
F = Dilution Factor
P = Potency of the standard in percentage
Page 5 of 6

Sign. & Date
07. Revision History
Document No. Version No. Date Reason
To update the detail procedure of analysis for Oxytetracycline

STP/RMA016 01 01.07.2018
Dihydrate BP
Page 6 of 6

Oxytetracycline Dyhydrate RMA016

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GENTRY PHARMACEUTICALS LTD.

Vangnahati, Sreepur, Gazipur.

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin

Section No. of Copy Received By (Signature & Date)

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin

Sl. No. Test Parameter Procedure BP

01. Appearance Yellow, crystalline powder.

B. To about 2 mg add 5 mL of sulfuric acid R. A deep red colour develops.

C. Dissolve about 10 mg in a mixture of 1 mL of dilute nitric acid R and 5 mL

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin

1.Tetrabutylammonium hydrogen sulphate solution :

2. Edetate disodium solution :

Dissolve 0.04 gm of edetate disodium in 100 ml of water. Ad just with 1 M

3. Phosphate buffer PH 7.5

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin

07. CHROMATOGRAPHIC SYSTEM :

Pu = Peak area of the sample.

P = Potency of standard in percentage.

C. ASSAY: BY SPECTROPHOTOMETRY METHOD:

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin

01. Std. Soln. : Dissolve 100 mg of Oxytetracycline Dihydrate WS in 60

02. Spl Soln. : Dissolve 100 mg of Oxytetracycline Dihydrate in 60 ml of

% Content of Oxytetracycline Dihydrate

Au = Absorbance of the Sample

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA016 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

Name Abdulla Al-Mamun Md. Kamrul Islam Mohammed Belal Uddin

07. Revision History

Document No. Version No. Date Reason

To update the detail procedure of analysis for Oxytetracycline

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