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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
Author(s) -
Favretto Donata,
Frison Giampietro,
Vogliardi Susanna,
Ferrara Santo Davide
Publication year - 2006
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2444
Subject(s) - chemistry , chromatography , buprenorphine , mass spectrometry , tandem mass spectrometry , electrospray ionization , liquid chromatography–mass spectrometry , ion trap , selected reaction monitoring , sample preparation in mass spectrometry , urine , direct electron ionization liquid chromatography–mass spectrometry interface , ion , ionization , chemical ionization , organic chemistry , opioid , biochemistry , receptor
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 d 4 ‐buprenorphine (d 4 ‐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 β ‐glucuronidase may be performed to distinguish between free and total BUP. Chromatographic separation is accomplished by gradient elution on a cyanopropyl 2.1 × 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. Copyright © 2006 John Wiley & Sons, Ltd.