High-speed analysis of residual solvents by flow-modulation gas chromatography

Rebecca E. Wittrig, Franklin Lewis Dorman, Jr., Christopher M. English, Richard D. Sacks

Research output: Contribution to journalArticle

15 Citations (Scopus)

Abstract

High-speed gas chromatographic (GC) separation of residual solvents in pharmaceutical preparations, using a flow-modulation technique, is described. These volatile compounds are separated on a series-coupled (tandem) column ensemble consisting of a polyethylene glycol column and a trifluoropropylmethyl/ dimethylpolysiloxane column. This column ensemble is operated in stop-flow mode to enhance, or "tune", the separation. A valve between the junction point of the tandem column ensemble and a source of carrier gas at a pressure above the GC inlet pressure is opened for intervals of 2-8s. This stops or slightly reverses the flow of carrier gas in the first column. Stop-flow pulses are used to increase the separation of target analytes that overlap in the total ensemble chromatogram, compared to non-stop-flow, or conventional, operation. All 36 target compounds, based on ICH Classes I and II residual solvent lists, are resolved in 12min using the stop-flow technique and a single chromatographic analysis.

Original languageEnglish (US)
Pages (from-to)75-82
Number of pages8
JournalJournal of Chromatography A
Volume1027
Issue number1-2
DOIs
StatePublished - Feb 20 2004

Fingerprint

Gas chromatography
Gas Chromatography
Gases
Modulation
Dimethylpolysiloxanes
Chromatographic analysis
Pressure
Chromatography
Pharmaceutical Preparations

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Biochemistry
  • Organic Chemistry

Cite this

Wittrig, Rebecca E. ; Dorman, Jr., Franklin Lewis ; English, Christopher M. ; Sacks, Richard D. / High-speed analysis of residual solvents by flow-modulation gas chromatography. In: Journal of Chromatography A. 2004 ; Vol. 1027, No. 1-2. pp. 75-82.
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High-speed analysis of residual solvents by flow-modulation gas chromatography. / Wittrig, Rebecca E.; Dorman, Jr., Franklin Lewis; English, Christopher M.; Sacks, Richard D.

In: Journal of Chromatography A, Vol. 1027, No. 1-2, 20.02.2004, p. 75-82.

Research output: Contribution to journalArticle

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AB - High-speed gas chromatographic (GC) separation of residual solvents in pharmaceutical preparations, using a flow-modulation technique, is described. These volatile compounds are separated on a series-coupled (tandem) column ensemble consisting of a polyethylene glycol column and a trifluoropropylmethyl/ dimethylpolysiloxane column. This column ensemble is operated in stop-flow mode to enhance, or "tune", the separation. A valve between the junction point of the tandem column ensemble and a source of carrier gas at a pressure above the GC inlet pressure is opened for intervals of 2-8s. This stops or slightly reverses the flow of carrier gas in the first column. Stop-flow pulses are used to increase the separation of target analytes that overlap in the total ensemble chromatogram, compared to non-stop-flow, or conventional, operation. All 36 target compounds, based on ICH Classes I and II residual solvent lists, are resolved in 12min using the stop-flow technique and a single chromatographic analysis.

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