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In the case of poisoning incidents that occur by pesticide ingestion, it has been required to determine the pesticide. First, screenings of pesticides using X-ray fluorescence spectroscopy (XRF), ion chromatography and gel-permeation chromatography were carried out. By XRF analysis, the elements of the active ingredient were detected in most pesticides, giving a first-step clue for estimating a compound. The proposed method was applied to estimate the pesticide in an actual fatal case. Second, an OASIS(R) MCX cartridge was used for the extraction of paraquat (PQ) and diquat (I)Q) from human blood, and their determination was carried out by capillary electrophoresis (CE). The recoveries of PQ and DQ from human plasma and whole blood were found to be above 87%. The proposed method was successfully applied to the determinations of PQ and DQ in human blood in actual cases. Third, a Titansphere(TM) TiO column was used for the extraction of phosphorus-containing amino acid-type herbicides (PAAHs) and their metabolites from human blood, and their determination was carried out by CE. The recoveries for glyphosate, aminomethylphosphonic acid, and glufosinate from human whole blood were found to be above 94%, and that for 3-methylphosphinicopropionic acid was 47%. The present method can be used for the rapid and simple determination of PAAHs in human blood in cases of accidental and suicidal ingestion.