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Ranitidine HCl Testing UV and HPLC Method

Ranitidine HCl Testing UV and HPLC Method Raw Material specification & analysis prescribes the requirements with UV Spectrophotometer spectrum and Alternate Method of Analysis on HPLC System and Other Testing procedures.

Ranitidine HCl Testing UV and HPLC Method and Purpose

This raw material specification & analysis prescribes the requirements for Ranitidine HCl raw material Testing UV and HPLC Method.

Characters

Ranitidine HCl Testing UV and HPLC Method is spread about 1.0 of sample on a clean, dry watch glass and observe the appearance, it should be white to pale yellow, crystalline, practically odorless powder. Is sensitive to light and moisture. Melts at about 140º, with decomposition.

Solubility

Ranitidine HCl Very soluble in water; sparingly soluble in alcohol.

Melting point

Melts at about 140º, with decomposition.

Grind the Ranitidine HCl sample into a fine powder in a mortar and pack the capillary tube with sample by tapping on a hard surface so as to form a tightly packed column of about 2.5mm to 3.5mm in height. Heat the melting point apparatus until the temperature is about 10 0C below the expected melting point and regulate the rate of rising of temperature at the rate of 1± 0.5 0C per minutes. Insert the capillary tube at around 5 0C below the expected melting point in heating vessel. Continue the heating and note down the temperature at which the sample melts with decomposition (at which frothing begins). It should be 140± 2 0C.

Identification (B)

Ultraviolet Absorption
Solution: 10 µg/ml
Medium: Distilled Water
Absorptivities at 229 nm and 315 nm, calculated on dried basis, do not differ by more than 3%.

Sample Preparation

Take 100mg Ranitidine hydrochloride TS in 100ml volumetric flask, dissolve them in 60ml water, stirrer for 10 min, made volume 100ml with water. Take 1ml and dilute to 100ml with water and measure absorbance at 314nm using water as a blank.

Standard Preparation

Take 100mg Ranitidine hydrochloride RS in 100ml volumetric flask, dissolve them in 60ml water, stirrer for 10 min, made volume 100ml with water. Take 1ml and dilute to 100ml with water and measure absorbance at 314nm using water as a blank.

Procedure

Observations and Calculations
Sample absorbance at 315nm = A
Standard absorbance at 315nm = B
Difference % = 100 – (Xx 100 /Y) = C%
Sample absorbance at 229nm = X
Standard absorbance at 229nm = Y
Difference % = 100 – (X x 100 / Y) = Z%
Limit:- Absorptivities at 229 nm and 315nm, calculated on dried basis, do not differ by more than 3%.

Identification (C)

A solution of it meets the requirements of the tests for Chloride
Solutions of chlorides yield with silver nitrate TS a white, curdy precipitate that is in soluble in nitric acid but is soluble in a slight excess of 6 N ammonium hydroxide.

pH

Between 4.5 and 6.0, in a solution (1 in 100)
Procedure: Take about 1 g of Ranitidine HCl, accurately weighed, into a 100 ml volumetric flask, and dissolve it in 100 ml with the distilled water. Take the solution into a clean and dried 50 ml beaker. Check the temperature of the solution. It should be 25 ± 2 °C. If not adjust the temperature by cooling or by heating as necessary. Not down the pH of the sample solution using pH meter.

Loss on drying

Dry it in vacuum at 60 0C for 3 hours: it loses not more than 0.75% of its weight.
Procedure: Take a clean and dry wide mouth weighing bottle that has been dried at 105± 2 0C in vacuum for 30 minutes and cool to room temperature in a desiccator then weigh it (W1). Transfer about 1 grams of sample into the weighing bottle. Weigh the bottle and note down the weight(W2). Calculate the net weight of the sample (W2-W1). Gently shake the bottle to distribute the material evenly. Place the weighing bottle in vacuum oven. Remove the stopper and keep it by the side of the weighing bottle or petridish. Close the oven, apply vacuum for about 3 hours. Stop vacuum, allow the air to enter the oven slowly. Open the chamber and close the weighing bottle promptly with stopper. Weigh the bottle and note down the weight W3. Calculate the % loss on drying using the formula.
% of Loss on Drying = W2-W3 x 100
                                      W2-W1

Ranitidine HCl Testing UV and HPLC Method

Assay (by HPLC)

Ranitidine HCl Testing UV and HPLC Method

Phosphate buffer

Place approximately 1900 ml of water in a 2.0 liter volumetric flask, accurately add 6.8 ml of phosphoric acid, and mix. Accurately add 8.6 ml of 50% sodium hydroxide solution, and dilute with water to volume. If necessary, adjust with 50% sodium hydroxide solution or phosphoric acid to a pH of 7.1, and filter.

Solution A
Prepare a mixture of Phosphate buffer and acetonitrile (98:2).

Solution B
Prepare a mixture of Phosphate buffer and acetonitrile (78:22).

Mobile phase
Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary.
Diluent
Use solution A

Standard preparation

Transfer about 25 mg of Ranitidine hydrochloride RS, accurately weighed, to a 200 ml volumetric flask. Dissolve in and dilute with Diluent to volume, and mix. Filter this solution through 0.45μm filter paper

Sample preparation

Transfer about 25 mg of Ranitidine hydrochloride TS, accurately weighed, to a 200 ml volumetric flask. Dissolve in and dilute with Diluent to volume, and mix. Filter this solution through 0.45μm filter paper.

Chromatographic Conditions

Column = 4.6 mm x 10 cm packing L1 that is stable from pH 1 to 12.
Column temperature= 35º
Detector = 230 nm
Flow Rate = 1.5 ml per minute
Inject Volume = 10 μl
Relative standard deviation for replicate injections is not more than 1.0%

Time                Solution A                 Solution B                  

(minutes)                (%)                           (%)                          Elution

0-10                   100—–0                     0——100               Linear gradient

10-15                       0                                 100                     Isocratic

15-16                   0——100                  100—–0                 Linear gradient

16-20                      100                                0                        re-equilibration

Procedure

Separately Inject equal volumes (about 10 μl) of the standard preparation and sample preparation into chromatograph, record the chromatograph and measure the area under the major peaks
Observations and Calculations

Area of major peak of sample preparation determination = A1
Area of major peak of standard preparation = A2
Concentration of sample preparation = C1
Concentration of standard preparation = C2
Ranitidine HCl % = A1x C2 x100/A2 x C1
Limit: – 97.5—102.0% (on dried basis)

Assay (by UV)

In-house method

Sample Preparation

Take 100mg Ranitidine hydrochloride TS in 100ml volumetric flask, dissolve them in 60ml water, stirrer for 10 min, made volume 100ml with water. Take 1ml and dilute to 100ml with water and measure absorbance at 314nm using water as a blank.

Standard Preparation

Take 100mg Ranitidine hydrochloride RS in 100ml volumetric flask, dissolve them in 60ml water, stirrer for 10 min, made volume 100ml with water. Take 1ml and dilute to 100ml with water and measure absorbance at 314nm using water as a blank.

Observations and Calculations
Sample absorbance at 315nm = X
Standard absorbance at 315nm = Y
Ranitidine HCl % = X x 100 / Y = Z%
Limits: 97.5—102.0% (on dried basis)

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