TY - JOUR
T1 - High-speed analysis of residual solvents by flow-modulation gas chromatography
AU - Wittrig, Rebecca E.
AU - Dorman, Frank L.
AU - English, Christopher M.
AU - Sacks, Richard D.
PY - 2004/2/20
Y1 - 2004/2/20
N2 - 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.
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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U2 - 10.1016/j.chroma.2003.10.046
DO - 10.1016/j.chroma.2003.10.046
M3 - Article
C2 - 14971486
AN - SCOPUS:0346654090
SN - 0021-9673
VL - 1027
SP - 75
EP - 82
JO - Journal of Chromatography A
JF - Journal of Chromatography A
IS - 1-2
ER -