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We examined the use of high resolution gas chromatography-electron ionization high resolution mass spectrometry (HRGC/EI-HRMS) in determining the toxaphene homologue distribution. Operating parameters such as electron energy, trap current and source temperature were optimized in order to obtain the maximum signal of the [M–C]+ and [M–HCl]+• fragment ions of each homologue group. Internal interferences due to the fragment ions from the homologues with one and two additional chlorine atoms were eliminated using EI-HRMS at a resolving power of 10 000 or higher. Tandem mass spectrometry (EI-MS/MS) was used in the fragmentation studies. HRGC/EI-HRMS-selected ion monitoring (SIM) at a resolving power of 10 000 was used to determine the homologue distribution of a commercial toxaphene mixture. This technique gave detection limits of ppb level. The performance of HRGC/EI-HRMS-SIM was compared to HRGC/ECNI-MS using isobutane as a moderating gas.
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Santos et al. (1997) studied this question.
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