STP Doxycycline Hyclate RMA009

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

STANDARD TEST PROCEDURE OF RAW MATERIAL-ACTIVE INGREDIENT
Name of Material DOXYCYCLINE HYCLATE BP
Document No.: STP/RMA009 Revision No. 01 Superseded No.: 01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/RMA004]
2. Specimen COA
DISTRIBUTION LIST
Section No. of Copy Received By (Signature & Date)
QC Laboratory 01
WITHOUT PERMISSION FROM HEAD OF QUALITY ASSURANCE OR HIS/HER Page 1 of 6

DELEGATE, COPY OF THIS DOCUMENT IS STRICTLY PROHIBITED

Sign. & Date
Sl. No. Test Parameters Test Procedures (BP)
1. Appearance Yellow, hygroscopic, crystalline powder.
Freely soluble in water and in methanol, sparingly soluble in ethanol (96 per
2. Solubility
cent). It dissolves in solutions of alkali hydroxides and carbonates.
B. To about 2 mg add 5 mL of sulfuric acid R. A yellow colour develops.
C. It gives reaction (a) of chlorides.
A. Dissolve in 2 ml of water R a quantity of the substance to be examined
equivalent to about 2 mg of chloride (Cl–) or use 2 ml of the prescribed
solution. Acidify with dilute nitric acid R and add 0.4 ml of silver nitrate
3. Identification solution R1. Shake and allow tostand. A curdled, white precipitate is formed.
Centrifuge and wash the precipitate with three quantities, each of 1 ml, of
water R. Carry out this operation rapidly in subdued light, disregarding the
fact that the supernatant solution may not become perfectly clear. Suspend
the precipitate in 2 ml of water R and add 1.5 ml of ammonia R. The
precipitate dissolves easily with the possible exception of a few large
particles which dissolve slowly.
2.0 to 3.0.
04 P H
Dissolve 0.1 g in carbon dioxide-free water R and dilute to 10 mL with the
same solvent.
Page 2 of 6
WITHOUT PERMISSION FROM HEAD OF QUALITY ASSURANCE OR HIS/HER

Sign. & Date
05 Water 1.4 per cent to 2.8 per cent, determined on 1.20 g.
06 Assay 95.0 per cent to 102.0 per cent of C22H25ClN2O8 (Anhydrous and ethanol-free
Substance).
A. ASSAY: BY HPLC METHOD
PROCEDURE:
01.Tetrabuylammonium hydrogen Sulphate solution:
Dissolve 1 gm of tetrabutylammonium hydrogen Sulphate in 100 ml of water.
Adjust with 1M sodium hydroxide to PH 8.
02.Edetate Disodium solution:

Dissolve 0.04 gm of Edetate Disodium in 100 ml of water. Adjust with 1M
sodium hydroxide to PH of 8.
03.Phosphate buffer PH 8 :
Mix 50.0 ml of 0.2 M Potassium Hydrogen phosphates with 46.80 ml of 0.2 M
Sodium Hydroxide solution and dilute to 200 ml with water.
04. Mobile Phase: Weigh 60.0 g of 2- methyl-2-propanol and transfer to 100

ml volumetric flask with the aid of 200 ml of water; add 400 ml of buffer
solution PH 8.0, 50 ml of a 10 g/l solution tetrabutylammonium Hydrogen
Sulphate. Adjust to PH 8.0 with dilute sodium hydroxide solution and 10 ml of
a 40g /l solution of sodium edetate adjusted to P H 8.0 with dilute sodium
hydroxide solution; dilute to 1000 ml with water.
05. Std. Solution:
Dissolve 20 mg of Doxycycline Hyclate WS in 0.1 M Hydrochloric Acid. Dilute

to 25 ml with the same solvent.
Page 3 of 6

Sign. & Date
06. Spl. Solution:

Dissolve 20 mg of Doxycycline Hyclate in 0.1 M Hydrochloric Acid. Dilute to
25 ml with the same solvent.
07. CHROMATOGRAPHIC SYSTEM:

a. Column : 4.6 mm ×250 mm. Packing L21
b. Detective wave length : 254 nm
c. Flow rate : 1ml / min.
d. Injection volume : 20 µl
e. RSD : NMT 1.0%
08. Separately inject equal volumes of Std. Solution and Spl. Solution into
Chromatograph. Record the Chromatograms and measure the peak
responses for the major peaks. Calculate the content by the formula:
% Content of Doxycycline Hydrochloride,
PU WS P
= --------- ´ --------- ´ F ´ -------- ´ 100
PS WU 100
Here,
PU = Peak area of the Sample
PS = Peak area of the Standard
WU = Weight of the Sample
Page 4 of 6

Sign. & Date
WS = Weight of the Standard

F = Dilution factor
P = Potency of the Standard used in percentage
B. ASSAY: BY SPECTROPHOTOMETRY METHOD:
1. Std. Solution: Dissolve 50 mg of Doxycycline Hyclate WS in 60ml of

0.1M Hydrochloric Acid and dilute to 100 ml with the same solvent.
Dilute 2 ml of the resulting solution to 100 ml with 0.1M Hydrochloric
acid.
2. Spl. Solution: Take 50 mg of Doxycycline Hyclate and dissolve in 60 ml

of 0.1M Hydrochloric Acid and dilute to 100 ml with the same solvent.
Dilute 2 ml of the resulting solution to 100 ml with 0.1M Hydrochloric
acid.
3. Measure the absorbances for the Standard and Sample solutions at 266
nm against blank. Calculate the content by the formula:
% Content of Doxycycline Hydrochloride

Au WS P
= --------- ´ --------- ´ F ´ -------- ´ 100
As Wu 100
Here,
Au = Absorbance of the Sample
AS = Absorbance of the Standard
Wu = Weight of the Sample
Page 5 of 6

Sign. & Date
Ws = Weight of the Standard

F = Dilution factor
P = Potency of the Standard used in percentage
07. Revision History
Document No. Version No. Date Reason
To update the detail procedure of analysis for Doxycycline

STP/RMA009 01 01.07.2018
Hyclate BP
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GENTRY PHARMACEUTICALS LTD.

Vangnahati, Sreepur, Gazipur.

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA009 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)

WITHOUT PERMISSION FROM HEAD OF QUALITY ASSURANCE OR HIS/HER Page 1 of 6

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA009 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 Parameters Test Procedures (BP)

1. Appearance Yellow, hygroscopic, crystalline powder.

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA009 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

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

05 Water 1.4 per cent to 2.8 per cent, determined on 1.20 g.

02.Edetate Disodium solution:

04. Mobile Phase: Weigh 60.0 g of 2- methyl-2-propanol and transfer to 100

05. Std. Solution:

Dissolve 20 mg of Doxycycline Hyclate WS in 0.1 M Hydrochloric Acid. Dilute

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA009 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

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

06. Spl. Solution:

07. CHROMATOGRAPHIC SYSTEM:

% Content of Doxycycline Hydrochloride,

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA009 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

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

WS = Weight of the Standard

1. Std. Solution: Dissolve 50 mg of Doxycycline Hyclate WS in 60ml of

2. Spl. Solution: Take 50 mg of Doxycycline Hyclate and dissolve in 60 ml

% Content of Doxycycline Hydrochloride

QUALITY ASSURANCE DEPARTMENT

Document No.: STP/RMA009 Revision No. 01 Superseded No.: 01

Prepared by Checked by Approved by

Sign. & Date

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

Ws = Weight of the Standard

07. Revision History

Document No. Version No. Date Reason

To update the detail procedure of analysis for Doxycycline

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