1st Edition

Measuring Elemental Impurities in Pharmaceuticals A Practical Guide

By Robert Thomas Copyright 2018
    502 Pages
    by CRC Press

    502 Pages
    by CRC Press

    Recent regulations on heavy metal testing have required the pharmaceutical industry to monitor a suite of elemental impurities in pharmaceutical raw materials, drug products and dietary supplements. These new directives s are described in the new United States Pharmacopeia (USP) Chapters <232>, <233>, and <2232>, together with Q3D, Step 4 guidelines for elemental impurities, drafted by the ICH (International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use), a consortium of global pharmaceutical associations, including the European Pharmacopeia (Ph.Eur.), the Japanese Pharmacopeia (JP) and the USP. This book provides a complete guide to the analytical methodology, instrumental techniques and sample preparation procedures used for measuring elemental impurities in pharmaceutical and nutraceutical materials.

    It offers readers the tools to better understand plasma spectrochemistry to optimize detection capability for the full suite of elemental PDE (Permitted Daily Exposure) levels in the various drug delivery categories. Other relevant information covered in the book includes:

    • The complete guide to measuring elemental impurities in pharmaceutical and nutraceutical materials.
    • Covers heavy metals testing in the pharmaceutical industry from an historical perspective.
    • Gives an overview of current USP Chapters <232> <233> and <2232> and ICH Q3D Step 4 Guidelines.
    • Explains the purpose of validation protocols used in Chapter <233>, including how J-values are calculated
    • Describes fundamental principles and practical capabilities of ICP-MS and ICP-OES.
    • Offers guidelines about the optimum strategy for risk assessment
    • Provides tips on how best to prepare and present your data for regulatory inspection.

    An indispensable resource, the fundamental principles and practical benefits of ICP-OES and ICP-MS are covered in a reader-friendly format that a novice, who is carrying out elemental impurities testing in the pharmaceutical and nutraceutical communities, will find easy to understand.

    Table of Contents




    Author Bio:

    Chapter 1: Testing for Heavy Metals: An ACS Perspective

    Chapter 2: Elemental impurities in Pharmaceuticals: An Overview

    Chapter 3: An Overview of ICP Mass Spectrometry

    Chapter 4: Principles of Ion formation

    Chapter 5: Sample Introduction

    Chapter 6: Plasma Source

    Chapter 7: Interface Region

    Chapter 8: Ion-Focusing System

    Chapter 9: Mass Analyzers: Quadrupole Technology

    Chapter 10: Mass Analyzers: Double-Focusing Magnetic Sector Technology

    Chapter 11: Mass Analyzers: Time-Of-Flight Technology

    Chapter 12: Mass Analyzers: Collision/Reaction Cell and Interface Technology

    Chapter 13: Ion Detectors

    Chapter 14: Peak Measurement Protocol

    Chapter 15: Methods of Quantitation

    Chapter 16: Review of ICP-MS Interferences

    Chapter 17: Routine Maintenance

    Chapter 18: Collecting and Preparing the Sample for Analysis

    Chapter 19: Sample Digestion Techniques for Pharmaceutical Samples

    Chapter 20: Performance and Productivity Enhancement Techniques

    Chapter 21: Coupling ICP-MS with Chromatographic Separation Techniques for Speciation Studies

    Chapter 22: Fundamental Principles, Method Development and Operational Requirements of ICP-OES

    Chapter 23: What Atomic Spectro-scopic Technique is Right for Your Lab?

    Chapter 24: Do You Know What it Costs to Run your Atomic Spectroscopy Instrumentation?

    Chapter 25: The Risk Assessment Approach

    Chapter 26: Regulatory Inspection Readiness

    Chapter 27: How to Select an ICP Mass Spectrometer: Some Important Analytical Considerations

    Chapter 28: Plasma Spectrochemistry Glossary of Terms

    Chapter 29: Useful Contact Information



    Robert J. Thomas has worked in the field of trace element analysis for over 40 years, including 24 years for an ICP-MS manufacturer and 15 years as a principal of his own consulting company. He has served on the ACS (American Chemical Society) Reagent Chemical Committee for the past 17 years as leader of the elemental impurities task force where he has worked closely with the USP to align heavy metal testing procedures in analytical reagents with those of pharmaceutical materials. He has authored almost 100 publications on trace element analysis and written three textbooks on ICP-MS and related topics, including this new book, which focuses on the new global directives on elemental impurities in pharmaceutical materials and dietary supplements. He is currently editor and frequent contributor to the Atomic Perspectives Column in Spectroscopy Magazine. He has a graduate degree in Analytical Chemistry from the University of Wales in the UK and is a Fellow of the Royal Society of Chemistry (FRSC, and a Chartered Chemist (CChem