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Updated: Jun 1, 2026

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Published on: June 9, 2021
Analysis of USP Organic Volatile Impurities and Thirteen Other Common Residual Solvents by Static Headspace Analysis
1Analytical Research, R&D Services, Mallinckrodt Inc., P.O. Box 5439, Saint Louis, Missouri 63147-0339.
Abstract:
Static headspace gas chromatography was investigated for the analysis of residual solvents in size-limited samples. The advantages of improved limits of detection at low ppm levels and decreased sample size requirements were realized. This methodology allows the measurement of 18 common residual solvents in 6 min using 1 mg or less of sample. Greater recovery of analytes from pure dissolution solvents without the use of salts became possible when smaller preparations of samples were combined with the use of smaller vials. Rapid equilibration of the static headspace sample preparations was an additional benefit of this modification. Optimized chromatography was developed to take advantage of the shorter equilibration time and to increase instrument productivity.
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