Analytical Method Development (AMD) and Quality Control (QC) departments responsible for evaluating the extractable volume from single-dose and multi-dose containers during development, validation, and routine batch release.

3. Responsibilities

• Analytical Scientist: Conducts extractable volume tests and documents results.
• QC Analyst: Performs sample handling, measurement, and calculation under aseptic conditions.
• QA Executive: Reviews results and ensures compliance with USP/Ph. Eur. specifications.

4. Accountability

The Head of Analytical Method Development is accountable for ensuring validated extractable volume methods are implemented and followed per regulatory standards.

5. Procedure

5.1 Equipment and Materials

1. Calibrated class A graduated cylinder or volumetric pipette
2. WFI or relevant test solution
3. Sterile syringes and needles
4. Analytical balance (for density conversion if needed)

5.2 Test Preparation

1. Condition the test samples to room temperature (25 ± 2°C).
2. Use aseptic techniques when withdrawing contents.

5.3 Test Procedure

1. Invert the container and withdraw contents completely using a sterile syringe without introducing air bubbles.
2. Transfer the contents into a calibrated cylinder and record the volume extracted.
3. Repeat the test for a statistically significant number of samples (n=10 for single-dose units).
4. For multidose containers, measure volume after five repeated extractions to simulate routine use.

5.4 Acceptance Criteria

• Single-dose containers: Not less than 90% of the labeled volume
• Multidose containers: Not less than the labeled volume across all extractions
• Average and individual container volumes must meet compendial expectations

5.5 Calculations

1. Calculate % extractable volume using the formula:
   % Extractable Volume = (Measured Volume / Labeled Volume) × 100
2. Report mean, standard deviation, and range for test units.

5.6 Method Validation Parameters

1. Accuracy: Recovery between 98–102% with certified volume standards
2. Precision: RSD ≤ 2% for replicate volume measurements
3. Linearity: Demonstrated from 0.5 mL to 50 mL volumes
4. Robustness: Evaluate influence of angle of withdrawal, syringe type, and needle gauge

6. Abbreviations

• USP: United States Pharmacopeia
• Ph. Eur.: European Pharmacopoeia
• QA: Quality Assurance
• AMD: Analytical Method Development

7. Documents

1. Extractable Volume Test Log – Annexure-1
2. Calibration Certificate for Glassware – Annexure-2
3. Validation Summary Report – Annexure-3

8. References

• USP <697>: Volume in Containers
• Ph. Eur. 2.9.17: Extractable Volume of Parenterals
• ICH Q2(R1): Validation of Analytical Procedures

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name	Amit Sharma	Neelam Saxena	Sunita Reddy
Designation	Analytical Chemist	QA Reviewer	Head – AMD
Department	Analytical Method Development	QA	Analytical Method Development

11. Annexures

Annexure-1: Extractable Volume Test Log

Sample ID	Labeled Volume (mL)	Measured Volume (mL)	% Extracted	Status
INJ-271-01	5.0	4.8	96%	Pass

Annexure-2: Calibration Certificate for Glassware

Glassware	Nominal Volume	Observed Volume	Correction Factor	Status
Graduated Cylinder	10 mL	9.98 mL	-0.02 mL	Pass

Annexure-3: Validation Summary Report

The extractable volume method was validated for ampoules, vials, and prefilled syringes. Accuracy and precision were within acceptable limits. Method is suitable for development and routine testing as per USP and Ph. Eur. requirements.

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
21/05/2025	2.0	Updated with linearity and robustness parameters	Annual Review	Sunita Reddy
20/03/2022	1.0	Initial SOP Release	New SOP	QA Head