Procedure for Melting Point Determination

1) Purpose

The purpose of this SOP is to outline the procedure for determining the melting point of pharmaceutical substances using appropriate analytical techniques.

2) Scope

This SOP applies to all pharmaceutical substances within the facility that require melting point determination as part of quality control, following pharmacopeial guidelines and internal specifications.

3) Responsibilities

Quality Control (QC) Department: Responsible for performing melting point determination and ensuring compliance with this SOP.
Analytical Laboratory: Responsible for conducting analysis using suitable techniques and interpreting results accurately.

4) Procedure

4.1 Sample Preparation:
    4.1.1 Obtain representative samples of pharmaceutical substances requiring melting point analysis.
    4.1.2 Ensure samples are properly labeled with batch numbers, dates, and any other relevant information.
    4.1.3 Prepare samples by grinding or cutting to ensure uniform particle size and surface area.

4.2 Melting Point Apparatus Setup:
    4.2.1 Set up the melting point apparatus according to manufacturer instructions and method validation protocols.
    4.2.2 Calibrate the apparatus using standard reference substances with known melting points.
    4.2.3 Ensure the heating rate and detection parameters are set appropriately for accurate melting point determination.

4.3 Melting Point Determination:
    4.3.1 Load prepared samples into the melting point apparatus, ensuring proper placement and observation of sample behavior.
    4.3.2 Heat samples gradually while observing for the point at which melting begins and complete liquefaction occurs.
    4.3.3 Record the observed melting point range and any relevant observations (e.g., onset temperature, clear melting).

4.4 Verification and Repeat Testing:
    4.4.1 Verify melting point results by repeating the analysis with additional samples or under varied conditions.
    4.4.2 Compare results with historical data or reference standards to ensure consistency and accuracy.
    4.4.3 Document any discrepancies or deviations from expected melting point ranges.

4.5 Calculation and Documentation:
    4.5.1 Calculate and report the average melting point range based on repeated analyses and observations.
    4.5.2 Document all melting point determination procedures, apparatus settings, and results in the Melting Point Determination Report.
    4.5.3 Review and approve the documentation by QC Manager before releasing results.

5) Abbreviations, if any

QC: Quality Control

6) Documents, if any

Melting Point Determination Report
Instrument Calibration Records
Method Validation Protocol and Report

7) Reference, if any

USP General Chapter <741> – Melting Range
Pharmacopeial standards for melting point determination in pharmaceutical substances

8) SOP Version

Version 1.0