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Determination of diazepam and its metabolites in human urine by liquid chromatography/tandem mass spectrometry using a hydrophilic polymer column.
Rapid Commun Mass Spectrom. 2008 Aug; 22(15):2333-41.RC

Abstract

Diazepam and its major metabolites, nordazepam, temazepam and oxazepam, in human urine samples, were analyzed by liquid chromatography (LC)/tandem mass spectrometry (MS/MS) using a hydrophilic polymer column (MSpak GF-310 4B), which enables direct injection of crude biological samples. Matrix compounds in urine were eluted first from the column, while the target compounds were retained on the polymer stationary phase. The analytes retained on the column were then eluted into an acetonitrile-rich mobile phase using a gradient separation technique. All compounds showed base-peak ions due to [M+H]+ ions on LC/MS with positive ion electrospray ionization, and product ions were produced from each [M+H]+ ion by LC/MS/MS. Quantification was performed by selected reaction monitoring. All compounds spiked into urine showed method recoveries of 50.1-82.0%. The regression equations for all compounds showed excellent linearity in the range of 0.5-500 ng/mL of urine. The limits of detection and quantification for each compound were 0.1 and 0.5 ng/mL of urine, respectively. The intra- and inter-day coefficients of variation for all compounds in urine were not greater than 9.6%. The data obtained from actual determination of diazepam and its three metabolites, oxazepam, nordazepam and temazepam, in human urine after oral administration of diazepam, 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 available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

18618924

Citation

Umezawa, Hironobu, et al. "Determination of Diazepam and Its Metabolites in Human Urine By Liquid Chromatography/tandem Mass Spectrometry Using a Hydrophilic Polymer Column." Rapid Communications in Mass Spectrometry : RCM, vol. 22, no. 15, 2008, pp. 2333-41.
Umezawa H, Lee XP, Arima Y, et al. Determination of diazepam and its metabolites in human urine by liquid chromatography/tandem mass spectrometry using a hydrophilic polymer column. Rapid Commun Mass Spectrom. 2008;22(15):2333-41.
Umezawa, H., Lee, X. P., Arima, Y., Hasegawa, C., Marumo, A., Kumazawa, T., & Sato, K. (2008). Determination of diazepam and its metabolites in human urine by liquid chromatography/tandem mass spectrometry using a hydrophilic polymer column. Rapid Communications in Mass Spectrometry : RCM, 22(15), 2333-41. https://doi.org/10.1002/rcm.3613
Umezawa H, et al. Determination of Diazepam and Its Metabolites in Human Urine By Liquid Chromatography/tandem Mass Spectrometry Using a Hydrophilic Polymer Column. Rapid Commun Mass Spectrom. 2008;22(15):2333-41. PubMed PMID: 18618924.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of diazepam and its metabolites in human urine by liquid chromatography/tandem mass spectrometry using a hydrophilic polymer column. AU - Umezawa,Hironobu, AU - Lee,Xiao-Pen, AU - Arima,Yoshiko, AU - Hasegawa,Chika, AU - Marumo,Akemi, AU - Kumazawa,Takeshi, AU - Sato,Keizo, PY - 2008/7/12/pubmed PY - 2008/9/11/medline PY - 2008/7/12/entrez SP - 2333 EP - 41 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 22 IS - 15 N2 - Diazepam and its major metabolites, nordazepam, temazepam and oxazepam, in human urine samples, were analyzed by liquid chromatography (LC)/tandem mass spectrometry (MS/MS) using a hydrophilic polymer column (MSpak GF-310 4B), which enables direct injection of crude biological samples. Matrix compounds in urine were eluted first from the column, while the target compounds were retained on the polymer stationary phase. The analytes retained on the column were then eluted into an acetonitrile-rich mobile phase using a gradient separation technique. All compounds showed base-peak ions due to [M+H]+ ions on LC/MS with positive ion electrospray ionization, and product ions were produced from each [M+H]+ ion by LC/MS/MS. Quantification was performed by selected reaction monitoring. All compounds spiked into urine showed method recoveries of 50.1-82.0%. The regression equations for all compounds showed excellent linearity in the range of 0.5-500 ng/mL of urine. The limits of detection and quantification for each compound were 0.1 and 0.5 ng/mL of urine, respectively. The intra- and inter-day coefficients of variation for all compounds in urine were not greater than 9.6%. The data obtained from actual determination of diazepam and its three metabolites, oxazepam, nordazepam and temazepam, in human urine after oral administration of diazepam, are also presented. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/18618924/Determination_of_diazepam_and_its_metabolites_in_human_urine_by_liquid_chromatography/tandem_mass_spectrometry_using_a_hydrophilic_polymer_column_ L2 - https://doi.org/10.1002/rcm.3613 DB - PRIME DP - Unbound Medicine ER -