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 language | English (US) |
|---|---|
| Pages (from-to) | 75-82 |
| Number of pages | 8 |
| Journal | Journal of Chromatography A |
| Volume | 1027 |
| Issue number | 1-2 |
| DOIs | |
| State | Published - Feb 20 2004 |
All Science Journal Classification (ASJC) codes
- Analytical Chemistry
- Biochemistry
- Organic Chemistry
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