On-line coupling of supercritical fluid extraction with multidimensional microcolumn liquid chromatography/gas...

An on-line multidimensional supercritical fluid extraction/microcolumn liquid chromatography/capillary gas chromatography system (SFE/LC/GC) has been developed and applied to the quantitative determination of trace levels (parts per billion) of chlorpyrifos insecticide in grass field samples. This system provides all the advantages of an on-line multidimensional system, including increased resolving power, high sensitivity, quantitation, precision, and automation potential. Off-line analysis of the grass extracts by GC with an electron capture detector yielded a complex chromatogram from which it was difficult to quantitate the chlorpyrifos, but analysis of the extract by LC/GC yielded a simple chromatogram from which chlorpyrifos could be quantitated. On-line SFE/LC/GC resulted in reduced sample preparation with the grass extract being deposited directly on the LC microcolumn via an impactor interface, followed by the LC/GC separation. The reproducibility of the on-line SFE/LC/GC procedure was studied and found to yield a relative standard deviation of 10.8% for the determination of chlorpyrifos insecticide in grass field samples at a concentration of 160 ng/g. Using this method, the entire analysis including extraction, clean-up, and gas chromatography required less than 0.1 mL of organic solvent.