Selective determination of paraquat and diquat in blood by high-performance liquid chromatography and high-performance liquid chromatography/mass spectrometry

Shigetoshi Kage, Keiko Kudo, Sunao Fukushima, Noriaki Ikeda

Research output: Contribution to journalArticle

13 Citations (Scopus)

Abstract

Selective determination of paraquat (PQ) and diquat (DQ) in human whole blood was carried out by high-performance liquid chromatography (HPLC) combined with UV and with fast atom bombardment (FAB) mass spectrometry (MS). The blood sample was deproteinized with 10 % trichloroacetic acid. The drugs present in the supernatant were extracted using a Sep-Pak C18 cartridge and applied to a chromatograph. Isonicotinic acid was used as external standard. PQ and DQ were clearly separated by HPLC on an octadecyl-silica column with a mobile phase of distilled water containing 0.05 % trifluoroacetic acid, 0.05 % perfluoro-n-butyric acid and 0.1 % triethylamine. The calibration curves were linear in the range from 0.1 to 10 μg/ml. The lower limits of detection were 0.05 μg/ml for both PQ and DQ, and recoveries of the compounds were about 80 %. When the precision of the method was evaluated, the coefficients of variation were found to be within 10 %. Confirmation of PQ and DQ in blood was carried out by HPLC with FAB-MS using a mobile phase of distilled water containing 0.1 % trifluoroacetic acid, 0.1 % perfluorc-n-butyric acid and 1 % thioglycerol. This method proved most useful in accurately identifying PQ and DQ in blood from two men who committed suicide by ingesting the herbicides.

Original languageEnglish
Pages (from-to)34-41
Number of pages8
JournalJapanese Journal of Forensic Toxicology
Volume16
Issue number1
Publication statusPublished - Dec 1 1998

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Diquat
Paraquat
High performance liquid chromatography
Mass spectrometry
Mass Spectrometry
Blood
High Pressure Liquid Chromatography
Fast Atom Bombardment Mass Spectrometry
Trifluoroacetic Acid
Butyric Acid
Isonicotinic Acids
Atoms
Trichloroacetic Acid
Water
Herbicides
Silicon Dioxide
Suicide
Calibration
Limit of Detection
Recovery

All Science Journal Classification (ASJC) codes

  • Pathology and Forensic Medicine
  • Toxicology

Cite this

Selective determination of paraquat and diquat in blood by high-performance liquid chromatography and high-performance liquid chromatography/mass spectrometry. / Kage, Shigetoshi; Kudo, Keiko; Fukushima, Sunao; Ikeda, Noriaki.

In: Japanese Journal of Forensic Toxicology, Vol. 16, No. 1, 01.12.1998, p. 34-41.

Research output: Contribution to journalArticle

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