E15-29: Atomic Spectrometry

Atomic Spectrometry:  Applications of Elemental Analysis
in the Pharmaceutical Industry
One-Day Course

Dr. Timothy L. Shelbourn, Eli Lilly and Company, Indianapolis, IN
Dr. Michael DeLeon, SPECTRO Analytical Instruments, Mahwah, NJ

With the recent changes in compendia and regulatory requirements for control of elemental impurities in drug products using instrumental analysis, analytical capabilities to measure elements (atomic absorption, ICP-optical emission spectroscopy, ICP mass spectrometry, and X-ray fluorescence spectrometry ) are now a necessity for developing, manufacturing and marketing commercial drug products.

This short course introduces a comprehensive overview of elemental impurities regulatory standards and guidelines (including USP <232> and ICH Q3D).    Technical aspects of the major analytical techniques will be discussed with an emphasis on pharmaceutical applications and method validation practices.

This one-day course will benefit analysts, QA and QC managers, regulatory professionals, and researchers who develop or manufacture drug product.

1.  Introduction to Elemental Analysis in Pharmaceutical Products
     * Under what circumstances is atomic spectrometry applied?
     * Review of compendia (monographs and general chapters)
2.  An Overview of USP, EP and JP Elemental Impurities Standards 
3.  Introduction and Review of ICH Q3D
4.  Risk Assessments and Control Strategies for Elemental Impurities

5.  Analytical Techniques
     * Atomic Absorption (flame, graphite furnace, hydride generation, cold vapor)
     * X-ray Fluorescence
     * Inductively coupled plasma optical emission spectroscopy
     * Inductively coupled plasma mass spectrometry
6.  Analytical Method Validation

Case studies will be presented to illustrate several risk assessment and control strategy scenarios for elemental impurities in drug product.

Timothy L. Shelbourn
MS Chemistry, Roosevelt University, Chicago, Illinois 
MBA, Webster University, St. Louis, Missouri 
BS Agrulculture, University of Nebraska, Lincoln, Nebraska

Employment History: 
2003-Present Research Scientist, Pharmaceutical R&D, Eli Lilly and Company
1986-2003: Research Scientist, Corporate Technology Resources, Baxter Healthcare

2014-Present:  American Chemical Society, Atomic Spectroscopy Subject Matter Expert for SciMind web based education series on atomic spectroscopy

2005-Present:  United States Pharmacopeia, General Chapters Expert Committee member

Michael DeLeon, is an Applications Scientist for Spectro Analytical Instruments for their X-ray Fluorescence and Spark Optical Emission Spectroscopy products.  Dr. DeLeon’s academic career includes a wealth of experience in a variety of analytical techniques such as AFM, TEM, High Resolution XRD, XAS, NEFS, TEY, and SEM-XRF.  Much of his research during his time with the New Jersey Institute of Technology was conducted at the National Synchrotron Light Source in Brookhaven National Labs. His focus was on the analysis strongly correlated electronic systems. Michael has used a variety of thin layer deposition techniques such as Pulsed Laser Deposition (PLD) (Naval Research Laboratories) and Metal-Organic Chemical Vapor Deposition (MOCVD) (in the Centre National de la Recherche Scientifique) for the manufacture of thin films from single monolayer to large crystalline layers.

Dr. DeLeon’s professional career as an Applications Scientist for Spectro Analytical Instruments for the X-ray Fluorescence and Spark Optical Emission Spectroscopy products lines, he work closely with sales, marketing, research and development, product management, service, and, of course, a wide customer base.  The industries he has worked closely with include: pharmaceutical, consumer goods, petrochemical, geological, and various metals industries. Michael also participates in ASTM committees to further international standards and specifications crucial for the various industries we serve.