Use of an injection port for thermochemolysis-gas chromatography/mass spectrometry: rapid profiling of biomaterials.
A simple and direct approach was developed for thermochemolytic analysis of a wide range of biomolecules present in plant materials using an injection port of a gas chromatograph/mass spectrometer (GC/MS) and a novel solids injector consisting of a coiled stainless steel wire placed inside a modified needle syringe. Optimum thermochemolysis (or Thermally Assisted Hydrolysis/Methylation) was achieved by using a suitable methanolic solution of trimethylsulfonium hydroxide (TMSH) or tetramethylammonium hydroxide (TMAH) with an injection port temperature of 350 degrees C. Intact, methylated flavonoids, saccharides, phenolic and fatty acids, lignin dimers and diterpene resin acids were identified. Samples include tea leaves, hemicelluloses, lignin isolates and herbal medicines. Unexpected chromatographic results using TMAH reagent revealed the presence of intact methylated trisaccharides (658 Da) and structurally informative dimer lignin markers.
Shadkami
Farzad
F
Analytical Chemistry Group, Department of Chemistry, Memorial University of Newfoundland, St. John's, NL, Canada A1B 3X7. shadkami@mun.ca
Helleur
Robert
R
D002099:Cacao / Q000737:chemistry; D002392:Catechin / Q000032:analysis; D004867:Equipment Design; D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation* / Q000379:methods; D020902:Hypericum / Q000737:chemistry; D028221:Larix / Q000737:chemistry; D008031:Lignin / Q000032:analysis; D028223:Pinus / Q000737:chemistry; D010936:Plant Extracts / Q000032:analysis; D018515:Plant Leaves / Q000737:chemistry; D011134:Polysaccharides / Q000032:analysis; D000644:Quaternary Ammonium Compounds / Q000737:chemistry; D015203:Reproducibility of Results; D013452:Sulfonium Compounds / Q000737:chemistry; D013662:Tea / Q000737:chemistry; D013696:Temperature
D010936:Plant Extracts; D011134:Polysaccharides; D000644:Quaternary Ammonium Compounds; D013452:Sulfonium Compounds; D013662:Tea; C007916:hemicellulose; C076151:Kraft lignin; D002392:Catechin; C009581:trimethylsulfonium; D008031:Lignin; C027917:tetramethylammonium