title: Determination of piperazine in working atmosphere and in human urine using derivatization and capillary gas chromatography with nitrogen- and mass-selective detection.
abstract: A reliable routine method is presented for the determination of piperazine down to the sub-ppm level in aqueous solutions and in urine. The method includes a two-phase derivatization procedure with ethyl- or isobutyl chloroformate as the reagent, followed by a capillary gas chromatographic determination using nitrogen- or mass selective detection. The addition of ammonia ensured a quantitative recovery. Detection limits for piperazine in urine were ca. 20 ng/ml using nitrogen-selective and ca. 1 ng/ml with mass-selective detection. The calibration plots were linear in the investigated range, 100-10,000 ng/ml with nitrogen-selective and 30-3000 ng/ml with mass-selective detection. The precision was ca. 6% at a concentration of 300 ng/ml. Acid anhydrides were investigated as alternative reagents in the two-phase derivatization procedure, and heptafluorobutyric acid anhydride in aqueous solutions gave approximately 100% recovery. However, in urine the recoveries of the investigated acid anhydride derivatives were unsatisfactory.
mesh_terms: D000395:Air Pollutants, Occupational / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D007202:Indicators and Reagents; D000077489:Piperazine; D010879:Piperazines / Q000032:analysis* / Q000652:urine
chemical_list: D000395:Air Pollutants, Occupational; D007202:Indicators and Reagents; D010879:Piperazines; D000077489:Piperazine