SOP Guide for Pharma

Elixir Department: SOP for Limit Test for Chloride and Sulfates – V 2.0

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Elixir Department: SOP for Limit Test for Chloride and Sulfates – V 2.0

Standard Operating Procedure for Limit Test for Chloride and Sulfates in Elixir Formulations

Department Elixir Department
SOP No. SOP/ELX/223/2025
Supersedes SOP/ELX/223/2022
Page No. Page 1 of 7
Issue Date 11/04/2025
Effective Date 15/04/2025
Review Date 11/04/2026

1. Purpose

To establish a standard procedure for conducting the limit test for chloride and sulfates in elixir formulations using visual comparison against standard solutions as per pharmacopeial guidelines.

2. Scope

This SOP is applicable to the Quality Control Department for testing the presence and permissible levels of chloride and sulfate impurities in raw materials and finished elixir products.

3. Responsibilities

  • QC Analyst:
    • Carry out the test, prepare reagents, and record observations.
  • QC Supervisor:
    • Ensure use of appropriate glassware and calibrated instruments.
  • QA Officer:
    • Review and approve test results before batch release.

4. Accountability

The QC Head is accountable for the accurate execution of the limit test. The QA Head is responsible for compliance with regulatory acceptance criteria and product quality assurance.

See also  Elixir Department: SOP for Alcohol Strength Adjustment in Final Product - V 2.0

5. Procedure

5.1 Limit Test for

Chloride
  1. Reagents: Nitric acid (dilute), silver nitrate solution (0.1N), standard chloride solution (e.g., 0.05845% NaCl equivalent to 0.035% Cl).
  2. Take 10 mL of the test solution in a Nessler cylinder.
  3. Add 1 mL of dilute nitric acid followed by 1 mL of silver nitrate solution.
  4. Mix and allow to stand for 5 minutes in diffused light.
  5. Simultaneously, prepare a standard solution using the same procedure.
  6. Compare the opalescence visually. The test passes if the opalescence in the sample is not greater than that of the standard.

5.2 Limit Test for Sulfates

  1. Reagents: Hydrochloric acid (dilute), barium chloride solution, standard sulfate solution (e.g., 0.181% K2SO4 equivalent to 0.1% SO42-).
  2. Take 10 mL of the test solution in a Nessler cylinder.
  3. Add 1 mL of dilute hydrochloric acid and 1 mL of 10% barium chloride solution.
  4. Stir with a glass rod and allow to stand for 10 minutes.
  5. Prepare a standard sulfate solution similarly.
  6. Compare turbidity. The test passes if the turbidity in the test sample is not more intense than that of the standard.

5.3 Notes

  • All glassware must be scrupulously clean and free from contaminants.
  • Do not perform the test under direct sunlight or harsh lighting.
  • If color interferes, decolorize using activated charcoal (if applicable).

5.4 Acceptance Criteria

  1. Chloride: Not more than 0.035% w/v (or as per specification).
  2. Sulfates: Not more than 0.1% w/v (or as per specification).

5.5 Documentation

  1. Record observations in the Chloride and Sulfate Limit Test Logbook (Annexure-1).
  2. Attach reagent preparation records and standard preparation references in the batch file.

6. Abbreviations

  • SOP: Standard Operating Procedure
  • QC: Quality Control
  • QA: Quality Assurance
  • w/v: Weight per Volume

7. Documents

  1. Chloride and Sulfate Limit Test Logbook (Annexure-1)
  2. Glassware and Reagent Preparation Records
  3. Batch Manufacturing Record (BMR)

8. References

  • USP General Chapter <221> – Inorganic Impurities: Tests for Chloride and Sulfate
  • IP / BP / Ph. Eur. Monographs for Limit Tests
  • 21 CFR Part 211.160 – Laboratory Controls

9. SOP Version

Version: 2.0

10. Approval Section

Prepared By Checked By Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Chloride and Sulfate Limit Test Logbook

Date Batch No. Chloride Result Sulfate Result Pass/Fail Tested By Verified By
11/04/2025 ELX-0425-041 Pass Pass Pass Rajesh Kumar Sunita Reddy

Revision History:

Revision Date Revision No. Revision Details Reason for Revision Approved By
01/01/2024 1.0 Initial SOP Release New SOP Creation QA Head
11/04/2025 2.0 Revised reagent quantities and test time Regulatory Alignment QA Head
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