Pittcon - Trace level testing and validation

Dr Gyorgy Vas, Intertek Research Fellow, will present an update on pharmaceutical trace level method development and validation at Pittcon 2016.

Recent issues and associated product recalls have forced the pharmaceutical industry to develop and validate methods at the trace or ultra trace level which demand lower detection limits beyond previously defined genotoxic impurities limits (~1 ppm). It has been pointed out that the Pharmaceutical industry does not always have processes, protocols and the analytical methodology to deal with such issues on a routine or non-routine basis. 

Trace level components are most often related to packaging component(s) which are usually evaluated during extractable and leachable testing. The other significant area which requires trace level determination on a relatively routine basis is testing for genotoxic impurities. 

Working at trace level analysis, the quality and performance of the instruments are critical and usually, trace level analysis is achieved by using highly selective methodologies such as liquid chromatography mass spectrometry LC-MS) and tandem mass spectrometry (LC-MS/MS) with Multiple Reaction Monitoring (MRM).  Method development is important to the whole process and key method development steps (LC method) include:

  • Understand analyte properties and intended use of method
  • Devise initial LC Conditions
  • Develop adequate separation, 
  • Sample preparation procedures which may include suitable sample clean-up procedure based on physical and chemical properties of matrix
  • Determine method linearity, accuracy and precision
  • Final method optimization/ including robustness testing to challenge method and identify weak spots

In particular state-of-the-art sample preparation is also often required in the analytical workflow to help facilitate trace level determination. This can involve techniques such as the application of solventless sample preparation which can help to eliminate certain chemical interferences. Pre-concentration of samples perhaps by using solid phase microextraction (SPME) instead of static head-space. SPME uses a coated fiber which removes the compounds from the sample by absorption in the case of liquid coatings or adsorbtion in the case of solid coatings. Alternatively using a Twister® Stir Bar Sorptive Extraction device (SBSE) instead of solvent based re-extraction could offer advantages. Twister® is a magnetic stir bar that has been coated with a partitioning phase of polydimethylsiloxane (PDMS). While it is stirring in the sample solution it extracts organic components from aqueous or other liquid samples.

 

Pittcon 2016 Courses

Dr Vas has been invited lead instructor to instruct pharmaceutical colleagues peers as part of the Short Courses program at Pittcon®2016, New Orleans, USA: 

Trace Level Analytical Method Validation in Pharmaceutical and in Food Industry  

  • Course Number:126
  • Course Length:1 Day Course
  • Date:Thursday, March 9th, 2016
  • Start Time: 08:30 AM - 05:00 PM 
  • Find out more

This course discusses method validation of trace level components in the pharmaceutical industry. Conventional pharmaceutical method validation practices are not always applicable to trace level analyses. Working at trace level analysis the quality and performance of the instruments are critical and usually trace level analysis is achieved by using highly selective methodology such as mass spectrometry and tandem mass spectrometry, unlike conventional pharmaceutical practices. 

Solventless Sample Preparation Prior to Mass Spectrometric Analysis  

  • Course Number:128
  • Course Length:1 Day Course
  • Date:Thursday, March 10th, 2016
  • Start Time: 08:30 AM - 05:00 PM 
  • Find out more

The course will provide examples and practical guidances how to prepare samples on a solventless fashion and will focus on the benefits and the disadvantages of solventless sample preparation techniques. During the course different analytical application areas will be discussed such as pharmaceutical, environmental, polymer, food and packaging. The different aspects of automation and instrumentation will also be presented.

If you are interested in either of these topics, please contact us to request a course summary.

Meet our Expert

Dr. Gyorgy Vas is a Research Fellow at Intertek Whitehouse, New Jersey, USA. He currently specializes in solventless sample preparation techniques such as SPME and Stir Bar Sorptive Extraction. He is responsible for all trace level method development and validation projects supporting pharmaceutical products and medical devices. Dr. Vas received his M.Sc. in Analytical Chemistry from the University of Debrecen (Hungary) and his Ph.D. in mass spectrometry from the University of Eotvos (Hungary). He has published 18 research papers and has received the Johnson & Johnson Outstanding Analytical Scientist Award and the Philip B. Hoffman Research Award for developing trace level analytical methods. He previously worked for Johnson & Johnson and held various academic and industrial positions  performing mass research related to mass spectrometry.

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