TY - JOUR
T1 - Chemical reactions with nanogram quantities of compounds collected from gas chromatographic effluent
AU - Attygale, Athula B.
AU - Morgan, E. David
PY - 1984/5/4
Y1 - 1984/5/4
N2 - Structural information about compounds, which are only in nanogram quantities in a complex mixture, can be obtained with the aid of gas chromatography (GC). Individual compounds can be efficiently trapped from the GC effluent into glass capillaries and there treated with a variety of reagents before re-chromatography. Information for identification can be quickly obtained, to confirm or augment information from gas chromatography-mass spectrometry, such as presence of a functional group, position and geometry of double bonds, or conversion to a more useful derivative. The reagent solution (1 μl) is injected into the capillary, where it dissolves the trapped material, and after reaction, the whole solution is re-injected into a capillary column. The apparatus required is very simple, consisting of nothing more expensive than a GC outlet splitter, a microlite syringe with a fine needle and an on-column injector. Examples are given of epoxidation of alkenes, borohydride reduction of carbonyl compounds, bromination and formation of methyl esters. For solid substances, melting points can be determined with great accuracy. Many reactions are rapid and the transfers are near quantitative.
AB - Structural information about compounds, which are only in nanogram quantities in a complex mixture, can be obtained with the aid of gas chromatography (GC). Individual compounds can be efficiently trapped from the GC effluent into glass capillaries and there treated with a variety of reagents before re-chromatography. Information for identification can be quickly obtained, to confirm or augment information from gas chromatography-mass spectrometry, such as presence of a functional group, position and geometry of double bonds, or conversion to a more useful derivative. The reagent solution (1 μl) is injected into the capillary, where it dissolves the trapped material, and after reaction, the whole solution is re-injected into a capillary column. The apparatus required is very simple, consisting of nothing more expensive than a GC outlet splitter, a microlite syringe with a fine needle and an on-column injector. Examples are given of epoxidation of alkenes, borohydride reduction of carbonyl compounds, bromination and formation of methyl esters. For solid substances, melting points can be determined with great accuracy. Many reactions are rapid and the transfers are near quantitative.
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U2 - 10.1016/S0021-9673(01)93586-1
DO - 10.1016/S0021-9673(01)93586-1
M3 - Article
AN - SCOPUS:48549110466
SN - 0021-9673
VL - 290
SP - 321
EP - 330
JO - Journal of Chromatography A
JF - Journal of Chromatography A
IS - C
ER -