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Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair.
J Anal Toxicol. 2005 Oct; 29(7):616-26.JA

Abstract

A liquid chromatography-tandem mass spectrometry method was developed for the simultaneous quantification of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair. Drugs were extracted from all matrices by liquid-liquid extraction with 1-chlorobutane. Chromatography was achieved using a XTerra MS C18 column eluted with a mixture of methanol and formate buffer. Data were acquired using positive electrospray ionization and multiple reaction monitoring using one precursor ion/product ion transition per compound. Quantification was performed using 13 deuterated analogues. Further confirmation of the identity of the compounds was achieved through a second injection of positive samples, monitoring two transitions per compound. The limits of quantification for all benzodiazepines ranged from 1 to 2 ng/mL in blood, 10 to 25 ng/mL in urine, and 0.5 to 10 pg/mg in hair. Linearity was observed from the limit of quantification of each compound to 200 ng/mL, 1000 ng/mL, and 1000 pg/mg for blood, urine, and hair, respectively (r2 > 0.99). Precision for quality control samples, spiked at three concentrations, was calculated (CV < 20% in most cases). Extraction recoveries for the three matrices ranged from 25.1 to 103.8%, except for one compound (cloxazolam in urine). Ion suppression was studied for all matrices. The validated assay was applied to authentic blood, urine, and hair samples from forensic cases.

Authors+Show Affiliations

Federal Public Service Justice, National Institute of Criminalistics and Criminology, Brussels, Belgium. marleen.laloup@just.fgov.beNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

16419390

Citation

Laloup, Marleen, et al. "Validation of a Liquid Chromatography-tandem Mass Spectrometry Method for the Simultaneous Determination of 26 Benzodiazepines and Metabolites, Zolpidem and Zopiclone, in Blood, Urine, and Hair." Journal of Analytical Toxicology, vol. 29, no. 7, 2005, pp. 616-26.
Laloup M, Ramirez Fernandez Mdel M, De Boeck G, et al. Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair. J Anal Toxicol. 2005;29(7):616-26.
Laloup, M., Ramirez Fernandez, M. d. e. l. . M., De Boeck, G., Wood, M., Maes, V., & Samyn, N. (2005). Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair. Journal of Analytical Toxicology, 29(7), 616-26.
Laloup M, et al. Validation of a Liquid Chromatography-tandem Mass Spectrometry Method for the Simultaneous Determination of 26 Benzodiazepines and Metabolites, Zolpidem and Zopiclone, in Blood, Urine, and Hair. J Anal Toxicol. 2005;29(7):616-26. PubMed PMID: 16419390.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair. AU - Laloup,Marleen, AU - Ramirez Fernandez,Maria del Mar, AU - De Boeck,Gert, AU - Wood,Michelle, AU - Maes,Viviane, AU - Samyn,Nele, PY - 2006/1/20/pubmed PY - 2006/2/4/medline PY - 2006/1/20/entrez SP - 616 EP - 26 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 29 IS - 7 N2 - A liquid chromatography-tandem mass spectrometry method was developed for the simultaneous quantification of 26 benzodiazepines and metabolites, zolpidem and zopiclone, in blood, urine, and hair. Drugs were extracted from all matrices by liquid-liquid extraction with 1-chlorobutane. Chromatography was achieved using a XTerra MS C18 column eluted with a mixture of methanol and formate buffer. Data were acquired using positive electrospray ionization and multiple reaction monitoring using one precursor ion/product ion transition per compound. Quantification was performed using 13 deuterated analogues. Further confirmation of the identity of the compounds was achieved through a second injection of positive samples, monitoring two transitions per compound. The limits of quantification for all benzodiazepines ranged from 1 to 2 ng/mL in blood, 10 to 25 ng/mL in urine, and 0.5 to 10 pg/mg in hair. Linearity was observed from the limit of quantification of each compound to 200 ng/mL, 1000 ng/mL, and 1000 pg/mg for blood, urine, and hair, respectively (r2 > 0.99). Precision for quality control samples, spiked at three concentrations, was calculated (CV < 20% in most cases). Extraction recoveries for the three matrices ranged from 25.1 to 103.8%, except for one compound (cloxazolam in urine). Ion suppression was studied for all matrices. The validated assay was applied to authentic blood, urine, and hair samples from forensic cases. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/16419390/Validation_of_a_liquid_chromatography_tandem_mass_spectrometry_method_for_the_simultaneous_determination_of_26_benzodiazepines_and_metabolites_zolpidem_and_zopiclone_in_blood_urine_and_hair_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/29.7.616 DB - PRIME DP - Unbound Medicine ER -