ISSN:
1612-1112
Schlagwort(e):
Hexamethylenediisocyanate, HDI
;
Isophoronediisocyanate, IPDI
;
LC
;
MS
;
Biological monitoring
Quelle:
Springer Online Journal Archives 1860-2000
Thema:
Chemie und Pharmazie
Notizen:
Summary 1,6-Diaminohexane (DAH, 1,6-hexamethylene diamine) and isophorone diamine (IPDA) have been derivatized with trifluoroethyl chloroformate (TFECF) using a two-phase procedure. Tetradeuterated 1,6-diaminohexane (TDDAH) was used as the internal standard. Thermospray (TSP) and plasma spray (PSP) mass spectrometric monitoring of positive (TSP+ and PSP+) and negative (TSP- and PSP-) ions revealed that monitoring of TSP+ furnished ten times more sensitivity than TSP- and twenty times more than PSP+. The sensitivity was about the same for the TFECF derivatives of DAH and IPDA. For TSP+ and TSP- the relative abundance of the ions was greatly influenced by the repeller voltage. Human urine samples were spiked with DAH and IPDA at six different concentrations in the range of 2.5–20 μg/l. LC-SIM and TSP+ determinations were performed and the m/z=(M+1) +fragments of the DAH-TFECF (m/z=369 amu), IPDA-TFECF (m/z=423 amu) and TDDAH-TFECF (m/z=373 amu) derivatives were monitored. Linear calibration plots were obtained; the correlation coefficient was 0.995 for DAH derivatives. The overall precision for human urine spiked to a concentration of 5 μg/l of DAH and 25 μg/l of IPDA were 4% and 7%, respectively (n=5). The detection limits for the DAH-TFECF and IPDA-TFECF derivatives were at the 10 pg level.
Materialart:
Digitale Medien
URL:
http://dx.doi.org/10.1007/BF02269636
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