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Published on: July 12, 2013
Pharmaceutical cleaning validation using non-proximate large-area desorption electrospray ionization mass
Santosh Soparawalla1, Gary A Salazar, Richard H Perry
1Department of Chemistry, Purdue University, West Lafayette, IN 47907, USA.
Rapid Communications in Mass Spectrometry : RCM
|December 17, 2008
Summary
Desorption electrospray ionization (DESI) enables rapid pharmaceutical cleaning validation. This ambient ionization technique detects active pharmaceutical ingredients (APIs) on manufacturing surfaces at low levels, meeting industry standards.
Area of Science:
- Analytical Chemistry
- Mass Spectrometry
- Pharmaceutical Science
Background:
- Desorption electrospray ionization (DESI) is a versatile ambient ionization technique.
- Pharmaceutical cleaning validation requires sensitive and efficient methods for detecting residual active pharmaceutical ingredients (APIs).
- Current methods may involve extensive sample preparation, impacting analysis time and cost.
Purpose of the Study:
- To explore the utility of a non-proximate, large-area DESI system for pharmaceutical cleaning validation.
- To assess the sensitivity and speed of DESI for detecting multiple APIs on representative manufacturing surfaces.
- To determine if DESI can meet the stringent limits set by the pharmaceutical industry for residual API detection.
Main Methods:
- Development of a non-proximate, large-area DESI system with a 2.5 cm² sprayer.
- Integration of a transport tube for sampling APIs from stainless steel surfaces up to 1 meter from the mass spectrometer.
- Analysis of eight different APIs including neostigmine, acebutolol, amiloride, amiodarone, ibuprofen, montelukast, potassium clavulanate, and beta-estradiol.
Main Results:
- The developed DESI system successfully detected APIs at levels as low as 10-30 ng/cm².
- Detection limits easily satisfied general acceptable limits for pharmaceutical cleaning validation.
- Analysis of representative surfaces from API manufacturing equipment was achieved at a rate of 30 seconds per analysis.
Conclusions:
- The large-area DESI system offers a sensitive, rapid, and efficient method for pharmaceutical cleaning validation.
- This ambient ionization approach minimizes sample preparation, making it suitable for industrial applications.
- DESI technology meets and exceeds the requirements for detecting residual APIs in pharmaceutical manufacturing.
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