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Potentials of ion trap collisional spectrometry for liquid chromatography/electrospray ionization tandem mass spectrometry determination of buprenorphine and nor-buprenorphine in urine, blood and hair samples.
Rapid Commun Mass Spectrom. 2006; 20(8):1257-65.RC

Abstract

A liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method has been developed for the analysis of buprenorphine (BUP) and nor-buprenorphine (NBUP) in biological fluids. Analytes are isolated from urine and blood, after addition of d4-buprenorphine (d4-BUP) as internal standard, by solid-phase extraction. Preparation of hair involves external decontamination, mechanical pulverization, overnight incubation in acidic medium, and neutralization prior to extraction. Enzymatic hydrolysis with beta-glucuronidase may be performed to distinguish between free and total BUP. Chromatographic separation is accomplished by gradient elution on a cyanopropyl 2.1 x 150 mm column. Positive ion ESI and MS analyses are carried out in an ion trap mass spectrometer. The use of this mass analyzer allows effective collisional experiments to be performed on ESI-generated MH+ species. Abundant product ions are produced, which can be monitored together with precursor ions without losing sensitivity. Thus, assay selectivity is definitely increased with respect to LC/ESI-MS/MS methods in which only precursor ions are monitored. The method has good linearity (calibration curves were linear in the range 0.1-10 ng/mL in urine and blood, in the range 10-160 pg/mg in hair) and limits of detection of 0.05 ng/mL for both BUP and NBUP in blood and urine samples, of 4 pg/mg for both analytes in hair. Both intra- and inter-assay precision and accuracy were satisfactory at three concentrations studied: relative standard deviations were <13.7% in urine, <17.3% in blood, <17.8% in hair; percent deviation of the mean from the true value was always <10.5% in urine and blood, <16.1% in hair. The method can be used to determine both analytes in the urine and hair of drug addicts on replacement therapy, and in post-mortem blood specimens when there is suspicion of drug-related death.

Authors+Show Affiliations

Favretto D
Forensic Toxicology and Antidoping, University Hospital of Padova, Via Falloppio 50, I-35121 Padova, Italy.
Frison G
No affiliation info available
Vogliardi S
No affiliation info available
Ferrara SD
No affiliation info available

MeSH

Analgesics, OpioidBuprenorphineCalibrationChromatography, High Pressure LiquidGlucuronidaseHairHumansReference StandardsReproducibility of ResultsSolutionsSpectrometry, Mass, Electrospray IonizationTandem Mass Spectrometry

Pub Type(s)

Journal Article

Language

eng

PubMed ID

16550495

Citation

Favretto, Donata, et al. "Potentials of Ion Trap Collisional Spectrometry for Liquid Chromatography/electrospray Ionization Tandem Mass Spectrometry Determination of Buprenorphine and Nor-buprenorphine in Urine, Blood and Hair Samples." Rapid Communications in Mass Spectrometry : RCM, vol. 20, no. 8, 2006, pp. 1257-65.
Favretto D, Frison G, Vogliardi S, et al. Potentials of ion trap collisional spectrometry for liquid chromatography/electrospray ionization tandem mass spectrometry determination of buprenorphine and nor-buprenorphine in urine, blood and hair samples. Rapid Commun Mass Spectrom. 2006;20(8):1257-65.
Favretto, D., Frison, G., Vogliardi, S., & Ferrara, S. D. (2006). Potentials of ion trap collisional spectrometry for liquid chromatography/electrospray ionization tandem mass spectrometry determination of buprenorphine and nor-buprenorphine in urine, blood and hair samples. Rapid Communications in Mass Spectrometry : RCM, 20(8), 1257-65.
Favretto D, et al. Potentials of Ion Trap Collisional Spectrometry for Liquid Chromatography/electrospray Ionization Tandem Mass Spectrometry Determination of Buprenorphine and Nor-buprenorphine in Urine, Blood and Hair Samples. Rapid Commun Mass Spectrom. 2006;20(8):1257-65. PubMed PMID: 16550495.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Potentials of ion trap collisional spectrometry for liquid chromatography/electrospray ionization tandem mass spectrometry determination of buprenorphine and nor-buprenorphine in urine, blood and hair samples. AU - Favretto,Donata, AU - Frison,Giampietro, AU - Vogliardi,Susanna, AU - Ferrara,Santo Davide, PY - 2006/3/22/pubmed PY - 2007/8/7/medline PY - 2006/3/22/entrez SP - 1257 EP - 65 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 20 IS - 8 N2 - A liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method has been developed for the analysis of buprenorphine (BUP) and nor-buprenorphine (NBUP) in biological fluids. Analytes are isolated from urine and blood, after addition of d4-buprenorphine (d4-BUP) as internal standard, by solid-phase extraction. Preparation of hair involves external decontamination, mechanical pulverization, overnight incubation in acidic medium, and neutralization prior to extraction. Enzymatic hydrolysis with beta-glucuronidase may be performed to distinguish between free and total BUP. Chromatographic separation is accomplished by gradient elution on a cyanopropyl 2.1 x 150 mm column. Positive ion ESI and MS analyses are carried out in an ion trap mass spectrometer. The use of this mass analyzer allows effective collisional experiments to be performed on ESI-generated MH+ species. Abundant product ions are produced, which can be monitored together with precursor ions without losing sensitivity. Thus, assay selectivity is definitely increased with respect to LC/ESI-MS/MS methods in which only precursor ions are monitored. The method has good linearity (calibration curves were linear in the range 0.1-10 ng/mL in urine and blood, in the range 10-160 pg/mg in hair) and limits of detection of 0.05 ng/mL for both BUP and NBUP in blood and urine samples, of 4 pg/mg for both analytes in hair. Both intra- and inter-assay precision and accuracy were satisfactory at three concentrations studied: relative standard deviations were <13.7% in urine, <17.3% in blood, <17.8% in hair; percent deviation of the mean from the true value was always <10.5% in urine and blood, <16.1% in hair. The method can be used to determine both analytes in the urine and hair of drug addicts on replacement therapy, and in post-mortem blood specimens when there is suspicion of drug-related death. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/16550495/Potentials_of_ion_trap_collisional_spectrometry_for_liquid_chromatography/electrospray_ionization_tandem_mass_spectrometry_determination_of_buprenorphine_and_nor_buprenorphine_in_urine_blood_and_hair_samples_ DB - PRIME DP - Unbound Medicine ER -