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Determination of paraquat and diquat in human body fluids by high-performance liquid chromatography/tandem mass spectrometry.
J Mass Spectrom. 2004 Oct; 39(10):1147-52.JM

Abstract

Paraquat (PQ) and diquat (DQ) in human whole blood and urine were analyzed by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) with positive ion electrospray ionization (ESI). The compounds were extracted with Sep-Pak C18 cartridges from whole blood and urine samples containing ethyl paraquat as an internal standard. The separation of PQ and DQ was carried out using ion-pair chromatography with heptafluorobutyric acid in 20 mM ammonium acetate and acetonitrile gradient elution for successful coupling with MS. Both compounds formed base peaks due to [M-H]+ ions by HPLC/ESI-MS and the product ions produced from each [M-H]+ ion by HPLC/MS/MS. Selective reaction monitoring (SRM) showed much higher sensitivity for both body fluids. Therefore, a detailed procedure for the detection of compounds by SRM with HPLC/MS/MS was established and carefully validated. The recoveries of PQ and DQ were 80.8-95.4% for whole blood and 84.2-96.7% for urine. The calibration curves for PQ and DQ showed excellent linearity in the range of 25-400 ng ml(-1) of whole blood and urine. The detection limits were 10 ng ml(-1) for PQ and 5 ng ml(-1) for DQ in both body fluids. The intra- and inter-day precision for both compounds in whole blood and urine samples were not greater than 13.0%. The data obtained from the determination of PQ and DQ in rat blood after oral administration of the compounds are also presented.

Authors+Show Affiliations

Department of Legal Medicine, Showa University School of Medicine, 1-5-8 Hatanodai, Shinagawa-ku, Tokyo 142-8555, Japan.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

15468125

Citation

Lee, Xiao-Pen, et al. "Determination of Paraquat and Diquat in Human Body Fluids By High-performance Liquid Chromatography/tandem Mass Spectrometry." Journal of Mass Spectrometry : JMS, vol. 39, no. 10, 2004, pp. 1147-52.
Lee XP, Kumazawa T, Fujishiro M, et al. Determination of paraquat and diquat in human body fluids by high-performance liquid chromatography/tandem mass spectrometry. J Mass Spectrom. 2004;39(10):1147-52.
Lee, X. P., Kumazawa, T., Fujishiro, M., Hasegawa, C., Arinobu, T., Seno, H., Ishii, A., & Sato, K. (2004). Determination of paraquat and diquat in human body fluids by high-performance liquid chromatography/tandem mass spectrometry. Journal of Mass Spectrometry : JMS, 39(10), 1147-52.
Lee XP, et al. Determination of Paraquat and Diquat in Human Body Fluids By High-performance Liquid Chromatography/tandem Mass Spectrometry. J Mass Spectrom. 2004;39(10):1147-52. PubMed PMID: 15468125.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of paraquat and diquat in human body fluids by high-performance liquid chromatography/tandem mass spectrometry. AU - Lee,Xiao-Pen, AU - Kumazawa,Takeshi, AU - Fujishiro,Masaya, AU - Hasegawa,Chika, AU - Arinobu,Tetsuya, AU - Seno,Hiroshi, AU - Ishii,Akira, AU - Sato,Keizo, PY - 2004/10/7/pubmed PY - 2004/12/16/medline PY - 2004/10/7/entrez SP - 1147 EP - 52 JF - Journal of mass spectrometry : JMS JO - J Mass Spectrom VL - 39 IS - 10 N2 - Paraquat (PQ) and diquat (DQ) in human whole blood and urine were analyzed by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) with positive ion electrospray ionization (ESI). The compounds were extracted with Sep-Pak C18 cartridges from whole blood and urine samples containing ethyl paraquat as an internal standard. The separation of PQ and DQ was carried out using ion-pair chromatography with heptafluorobutyric acid in 20 mM ammonium acetate and acetonitrile gradient elution for successful coupling with MS. Both compounds formed base peaks due to [M-H]+ ions by HPLC/ESI-MS and the product ions produced from each [M-H]+ ion by HPLC/MS/MS. Selective reaction monitoring (SRM) showed much higher sensitivity for both body fluids. Therefore, a detailed procedure for the detection of compounds by SRM with HPLC/MS/MS was established and carefully validated. The recoveries of PQ and DQ were 80.8-95.4% for whole blood and 84.2-96.7% for urine. The calibration curves for PQ and DQ showed excellent linearity in the range of 25-400 ng ml(-1) of whole blood and urine. The detection limits were 10 ng ml(-1) for PQ and 5 ng ml(-1) for DQ in both body fluids. The intra- and inter-day precision for both compounds in whole blood and urine samples were not greater than 13.0%. The data obtained from the determination of PQ and DQ in rat blood after oral administration of the compounds are also presented. SN - 1076-5174 UR - https://www.unboundmedicine.com/medline/citation/15468125/Determination_of_paraquat_and_diquat_in_human_body_fluids_by_high_performance_liquid_chromatography/tandem_mass_spectrometry_ L2 - https://doi.org/10.1002/jms.695 DB - PRIME DP - Unbound Medicine ER -