Amlodipine Besylate Raw Material (API) is the best-prescribed Raw Material (API) for cardiovascular ailment main hazard element for high blood pressure. First mentioned low fee ultraviolet-seen method for the dedication and quantitation of medicine in prescription drugs and organic fluids. Chromatographic strategies have an utility with appreciate to hint evaluation. Different sorts of chromatography together with excessive-overall performance liquid chromatography, excessive overall performance skinny layer chromatography have maximum common packages withinside the subject of pharmaceutical in addition to biomedical analyses. Amlodipine Besylate Raw Material (API) Chromatography mixed with mass spectrophotometry has the capacity to acquire molecular ion.
Amlodipine Besylate Raw Material (STANDARD
ANALYTICAL PROCEDURE)
REFRENCE: USP 44, NF 39
APPROVAL BLOCK
| Title | Designation | Signature/Date |
| Written By: | Quality Control Analyst | |
| Reviewed By: | Quality Control Manager | |
| Verified By: | Quality Assurance In-charge | |
| Approved By: | Technical Operation Director |
1.0 PURPOSE:
To describes the procedure for testing of raw material Amlodipine Besylate
2.0 SCOPE:
This document describes the basic principles, defines the responsibilities and lays down the procedure for the analytical testing of Amlodipine Besylate.
3.0 RESPONSIBILITY:
QC Analyst is responsible for physical / chemical testing and preparing standard analytical procedure.
It is the responsibility of QC Manager to assist and ensure Testing Procedure as per SAP and to make certain that this SAP is followed in its entirety, reviewed regularly and revised as necessary.
4.0 REFERENCE:
USP 43, NF 38
5.0 MATERIAL AND EQIUPMENT:
- Analytical balance
- FTIR
- HPLC
- Hot Plate
- Vacuum Assembly
- pH Meter
- Muffle Furnace
- Spatula
- Sulphuric Acid
- Distilled Water
- Glassware
- Polarimeter
- Sodium Hydroxide
- Hydrochloric acid
- Methanol
- Triethylamine
- Phosphoric Acid
- Acetonitrile
- 2-Propanol
- Alcohol
6.0 PROCEDURE:
6.1 SAMPLING PLAN:
Take sample from each container and identify individually. Make representative sample and divide into two portions. 1st portion for remaining analysis and 2nd portion for keeping sample.
6.2 RETAIN SAMPLE:
Pack sufficient quantity of sample in polythene bag and seal in aluminium foil finally. Keep the sample at recommended storage conditions for at least 1 year after expiry/retest date.
6.3 RECORD KEEPING:
Analysis records including raw data generated during the application of this procedure will be kept at least one year after the expiry or one year after the last distribution whichever is longer.
6.4 DESCRIPTION:
6.4.1 SPECIFICATIONS:
White to almost white powder
6.4.2 PROCEDURE:
Spread approximately 2.0 g of the sample over the cleaned and dried petri dish and examine visually against white background. Check the appearance of color, nature and any visible foreign particles.
6.5 SOLUBILITY:
| Each gram of solute in mL of Solvent | Sparingly Soluble | From 30 To 100 | |
| Very Soluble | Less Than 1 | Slightly Soluble | From 100 To 1000 |
| Freely Soluble | From 1 To 10 | Very Slightly Soluble | From 1000 To 10000 |
| Soluble | From 10 To 30 | Practically Insoluble | More Than 10000 |
6.5.1 SPECIFICATIONS:
Freely soluble in Methanol, sparingly soluble in alcohol, slightly soluble in water and 2-propanol.
6.5.2 PROCEDURE:
Re Transfer accurately 1 g or the quantity specified in the test requirement, of the sample into precleaned, dried, stoppered test tube or Nessler cylinder.
Add an appropriate volume of the specified solvent. Determine the volume of the solvent. The solution should be clear and free from foreign particles.
6.6 IDENTIFICATION
6.6.1 SPECIFICATIONS:
Identification by HPLC & by FTIR
6.6.2 PROCEDURE:
6.6.2.1 By HPLC
The retention time of the major peak in the chromatogram of the test solution should correspond to that in the chromatogram of the standard solution, as obtained by HPLC method.
6.6.2.2 By FTIR:
Infrared absorption spectrum of the sample should be concordant with that of the standard
6.7 WATER: (By Karl Fischer)
6.7.1 SPECIFICATION:
Water Determination, = not more than 0.5%for the anhydrous form, If labeled as the hydrated form, the limit is between 3.1% and 5.0%.
6.7.2 PROCEDURE
Add about 20 mL of methanol to the titration vessel and neutralized it with K.F. reagent. Quickly add about 0.100 g of accurately weighed of the crushed sample, stir to dissolve and titrate to the electrometric end point with K.F. reagent. Record the water contents.
6.8 OPTICAL ROTATION
6.8.1 SPECIFICATIONS: -0.10º to +0.1º at 20 ºC
6.8.2 PROCEDURE:
Preparation of Sample solution: 10mg/mL in Methanol AR Grade Take reading on Polarimeter by using methanol as blank
Sample weight = A
Length of tube in decimeter=L
Specific rotation= Value x 50 x 100
A x L x 100-Water
6.9 RESIDUE ON IGNITION
6.9.1 SPECIFICATIONS:
NMT 0.2%. Determine on 1.0 g Use a platinum, Silica, quartz, crucible.
6.9.2 PROCEDURE:
Ignite a suitable crucible (Silica or quartz) at 600 ± 50 °C for 30 min, allow to cool in a desiccator over silica gel or other suitable desiccant and weigh. Place the prescribed amount of the substance to be examined in the crucible and weigh. Moisten the substance to be examined with a small amount of sulfuric acid R (usually 1 mL) and heat gently at as low a temperature as practicable until the sample is thoroughly charred. After cooling, moisten the residue with a small amount of sulfuric acid R (usually 1 mL), heat gently until white fumes are no longer evolved and ignite at 600 ± 50 °C until the residue is completely incinerated. Ensure that flames are not produced at any time during the procedure. Allow the crucible to cool in a desiccator over silica gel or other suitable desiccant, weigh it again and calculate the percentage of residue. Unless Otherwise specified, if the amount of residue so obtained exceeds the limit specified in the individual monograph, repeat the moistening with sulfuric Acid, Heating and igniting as before using a 30- minute ignition period, until two consecutive weighing of the residue do not differ by more than 0.5mg or until the percentage of residue complies with the limit in the individual Monograph. Calculate the percentage of residue by following formula;
% age Sulfated ash= Weight of Residue x 100
Weight of Sample Taken
Weight of empty Crucible =A
Weight of Crucible with Sample =B
Weight of Sample =C
Weight of Crucible with Sample after ignition= D=
Weight of Residue= D-A= E
Residue on Ignition (% w/w) = E x 100 / C
6.10 ASSAY
6.10.1 SPECIFICATIONS:
ACCEPTANCE CRITERIA: Amlodipine Besylate is anhydrous or hydrated and contains not less than 97.0 percent and not more than 102.0 percent of C20H25CIN2O5 C6H6O3S, calculated on the anhydrous basis.
6.10.2 pH 3.0 BUFFER:
Dissolve 7.0 mL of triethylamine in 800 mL of water. Adjust with phosphoric acid to a pH of 3.0 ± 0.1, and dilute with water to 1 L.
6.10.3 MOBILE PHASE:
Prepare a filtered and degassed mixture of pH 3.0 Buffer, methanol, and Acetonitrile (50:35:15). Make adjustments if necessary
6.10.4 STANDARD PREPARATION:
Dissolve an accurately weighed quantity of Amlodipine Besylate RS in Mobile phase to obtain a solution having a known concentration of about 0.05 mg per mL.
6.10.5 ASSAY PREPARATION:
Transfer about 50 mg of Amlodipine Besylate, accurately weighed, to a 50-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.
Transfer 5.0 mL of this solution to a 100 mL volumetric flask, dilute with Mobile phase to volume, and mix.
6.10.6 CHROMATOGRAPHIC SYSTEM:
Detection wavelength: 237nm
Column: C18 (3.9 mm × 150mm, 5μm)
Flow rate: 1.0 mL/min
Column temperature: 30℃
Injection Volume: 10 μL
PROCEDURE:
Separately inject equal volumes (about 10 μL)of the standard preparation and the assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks.
6.10.7 SYSTEM SUITABILITY:
6.10.7.1 RELATIVE STANDARD DEVIATION:
NMT 2.0 % for standard solution.
6.10.8 CALCULATIONS:
Average Area under Curve of Assay preparation x Standard dilution x Potency of standard
Average Area under Curve of Standard preparation x Sample dilution
6.10.9 RESULTS:
Amlodipine Besylate (on anhydrous basis) % age = Result % (as such) x 100
100- Water
6.10.10 STORAGE:
Preserve in tight containers, protected from light. Store at room temperature.
7 RISK ANALYSES:
EVIDENCE OF RECORDS & REFERENCES
USP44, NF39 Certificate of Analysis Raw Material
FORMAL KPIs (Key Performance Indicators)
Storage Condition Contamination of sampling tools