Procedure for Elemental Impurity Testing
1) Purpose
The purpose of this SOP is to outline the procedure for testing elemental impurities in pharmaceutical products to ensure compliance with safety and regulatory standards.
2) Scope
This SOP applies to all pharmaceutical products within the facility that require elemental impurity testing as part of quality control, following pharmacopeial guidelines and regulatory requirements.
3) Responsibilities
Quality Control (QC) Department: Responsible for performing elemental impurity testing and ensuring compliance with this SOP.
Analytical Laboratory: Responsible for conducting atomic absorption spectroscopy (AAS) or inductively coupled plasma (ICP) analysis and interpreting results.
4) Procedure
4.1 Sample Preparation:
4.1.1 Obtain representative samples of pharmaceutical products requiring elemental impurity analysis.
4.1.2 Ensure samples are properly labeled with batch numbers, dates, and any other relevant information.
4.1.3 Prepare samples according to specified procedures, including digestion or extraction methods suitable for elemental impurity detection.
4.2 Instrument Setup:
4.2.1 Prepare the AAS or ICP instrument according to manufacturer instructions and method validation protocols.
4.2.2 Ensure the instrument is calibrated using certified reference standards for elemental impurities.
4.2.3 Perform system suitability tests to verify instrument performance and analytical sensitivity.
4.3 Elemental Impurity Analysis: 4.4 Calibration and Standard Preparation: 4.5 Calculation of Results: 4.6 Quality Assurance and Validation: 4.7 Documentation: QC: Quality Control Elemental Impurity Testing Report USP General Chapter <232> – Elemental Impurities – Limits Version 1.0
4.3.1 Inject prepared samples into the AAS or ICP system using appropriate sample introduction techniques.
4.3.3 Collect analytical data and ensure accurate peak integration for quantification purposes.
4.4.1 Prepare calibration standards covering the required concentration range for elemental impurities.
4.4.2 Analyze calibration standards to generate calibration curves for each elemental impurity.
4.4.3 Validate calibration curves and adjust method parameters as necessary to ensure accuracy and linearity.
4.5.1 Calculate elemental impurity concentrations in sample solutions based on calibration curve data and sample dilutions.
4.5.2 Apply correction factors if applicable (e.g., for sample matrix effects, recovery efficiency).
4.5.3 Review results against acceptance criteria specified in pharmacopeial standards or internal specifications.
4.6.1 Document all instrumental parameters, sample preparations, and analytical results in the Elemental Impurity Testing Report.
4.6.2 Conduct method validation studies to demonstrate the accuracy, precision, specificity, and sensitivity of the elemental impurity testing method.
4.6.3 Review validation data and ensure compliance with regulatory requirements before releasing test results.
4.7.1 Record all elemental impurity testing procedures, chromatograms, calibration data, and interpretations in the Elemental Impurity Testing Report.
4.7.2 Maintain detailed records of sample details, instrument calibrations, method validations, and analyst training records.
4.7.3 Review and approve the documentation by QC Manager.5) Abbreviations, if any
AAS: Atomic Absorption Spectroscopy
ICP: Inductively Coupled Plasma6) Documents, if any
Instrument Calibration Records
Method Validation Protocol and Report7) Reference, if any
ICH Q3D – Elemental Impurities Guidelines for Pharmaceuticals8) SOP Version
