IDENTIFICATION OF DIFLUBENZURON BY PACKED-CAPILLARY SUPERCRITICAL-FLUID CHROMATOGRAPHY MASS-SPECTROMETRY WITH ELECTRON-CAPTURE NEGATIVE IONIZATION

被引:10
作者
BREDE, C [1 ]
LUNDANES, E [1 ]
机构
[1] UNIV OSLO,DEPT CHEM,N-0315 OSLO,NORWAY
关键词
D O I
10.1016/0021-9673(95)00299-3
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The thermolabile insecticide diflubenzuron [1-(4-chlorophenyl)-3-(2,6-difluorobenzoyl)urea] was successfully chromatographed by supercritical fluid chromatography on a 320 mu m I.D. Inertsil C-8 column using neat carbon dioxide as mobile phase. Detection and electron-capture negative ionization (ECNI) mass spectrometric characterization were accomplished using a double focusing mass spectrometer with a modified ion source and coaxial direct fluid introduction. Detection limits of 1.0 mu g/ml and 0.03 mu g/ml were obtained in full-scan and selected-ion monitoring (SIM) mode, respectively. The restrictor heater temperature was found to have a major influence on the signal intensity and fragmentation pattern, as thermal degradation was believed to take place or be initiated on the hot restrictor wall. The relative abundance of the molecular ion amounted to 100% using restrictor temperatures of 160 degrees C and 170 degrees C, while it was completely absent at 190 degrees C. At the lower temperatures, [M - HF](-.) was the most significant fragment ion.
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页码:95 / 101
页数:7
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