A screening method for the rapid detection of barbiturates in serum by means of tandem mass spectrometry

Brzezinka, H.; Bold, Peter; Budzikiewicz, H.

doi:10.1002/bms.1200220606

Cited by 7 publications

(4 citation statements)

References 8 publications

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“…Total ion chromatogram of (1) CID mass spectrum of protonated uracil, an analogous compound. There is also the appearance of an ion at m/z 42 (NCO À ), representing a fragmentation pattern reported previously by Sakurai et al 31 in the high energy CID mass spectrum derived from deprotonated uracil, and by Brzezinka et al 32 in the EI-MS/MS spectra of selected negatively charged barbiturates. There are other fragment ions observed as well: at m/z 85, which is derived from the loss of the part of the ring with the side chain attachment, and a minor fragment showing the loss of 85 u. Interestingly, the fragment at m/z 85 is derived from the fragmentation of the barbiturate ring with the negative charge residing at O 2 , suggesting that the negative charge can be carried on both O 2 and O 4 during the CID process, similar to results reported from the CID mass spectra of protonated uracil derivatives.…”

Section: Mass Spectra and Total Ion Chromatogramsmentioning

confidence: 84%

Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbital and thiopental in human serum

Spell

Srinivasan

Stewart

et al. 1998

Rapid Commun. Mass Spectrom.

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Four commonly used barbiturates (phenobarbital, butalbital, pentobarbital and thiopental) were analyzed in human serum using supercritical fluid extraction (SFE) and negative ionization LC/ESI-MS/MS. Barbital was used as the internal standard. Carbon dioxide SFE was performed at 40 degrees C and 500 atm, with a total extraction time of 35 min. The analytes were collected off-line in a liquid trap containing absolute methanol. Samples were then concentrated by vacuum centrifugation. The high performance liquid chromatography separation utilized gradient elution with a total analysis time of 21 min. The precursor and major product ions for the four barbiturates were monitored on a triple quadrupole mass spectrometer with negative ion electrospray ionization (ESI) in the multiple reaction monitoring mode as follows: (1) thiopental (m/z 241.20-->58.00), (2) phenobarbital (m/z 231.10-->188.0), (3) pentobarbital (m/z 225.10-->181.90) and (4) butalbital (m/z 222.80-->179.90). In the case of phenobarbital, pentobarbital and butalbital, the most abundant product ion arises from the loss of 43 u (HCNO loss). However, in the case of thiopental, the most abundant product ion was observed at m/z 58.0 (the [M-183]-ion, or NCS-). Mechanisms for the formation of the collision induced dissociation reaction products of these barbiturates are proposed.

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Section: Mass Spectra and Total Ion Chromatogramsmentioning

confidence: 84%

Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbital and thiopental in human serum

Spell

Srinivasan

Stewart

et al. 1998

Rapid Commun. Mass Spectrom.

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“…17 In another mass spectrometric screening method, the barbiturates were fragmented owing to the loss of HNCO under the electron impact conditions. 18 Using the ion mobility mass spectrometry with desorption electrospray ionization source, barbituric acid was found only in the negative mode. 19…”

Section: Introductionmentioning

confidence: 99%

Investigation of corona discharge ionization of barbituric acid using ion mobility spectrometry along with quantum chemical calculations

Ghahremani

Salehabadi

Bahrami

et al. 2021

Eur J Mass Spectrom (Chichester)

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This study aimed at examining atmospheric-pressure chemical ionization of barbituric acid through the corona discharge ion mobility spectrometry (CD-IMS) and the quantum chemical calculations. The results indicated two product ion peaks in the IMS spectrum of barbituric acid. The thermal decomposition of the barbituric acid sample was investigated by scanning the temperature of the injection port and analyzing the temporal evolution of the IMS peaks over elapsed time. It was found that the barbituric acid sample was not thermally decomposed in the injection port of the instrument. Experimental evidences were collected by changing the reactant ions, concentration of barbituric acid sample, and IMS cell temperature. The two observed peaks were then assigned to cationic form and oxygen protonated isomers of barbituric acid. The positions of the product ion peaks were explicated considering the dipole moments of the product ions.

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“…In tandem mass spectrometry (MS/MS) the mass spectrometer serves both as separation device and as a tool for structure elucidation [5]. Using the ionization technique of fast atom bombardment (FAB) the drugs and their polar metabolites present in urine or other biological matrices (e.g., serum) can be identified directly and characterized without extensive sample work-up [7,8].…”

Section: Introductionmentioning

confidence: 99%

A fast screening method for tricyclic antidepressants and their urinary metabolites by FAB‐tandem mass spectrometry

Schäfer¹,

Budzikiewicz²,

Brzezinka³

et al. 1997

Journal of Spectroscopy

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A screening method for tricyclic antidepressants (TCA) and their urinary metabolites by FAB tandem mass spectrometry (FAB MS/MS) is presented. The collision induced dissociation (CID) behavior of pure dibenzocycloheptadienes (amitriptyline1, nortriptyline2), dibenzoxepines (doxepine3, dosulepine4), dibenzazepines (imipramine5, desipramine6, trimipramine7) and the iminostilbene derivative opipramol8is described and used for the specific determination of these tricyclics by MS/MS.For the screening procedure a methanolic extract of the urine sample is passed through a XAD-2 column and the eluate is examined without further purification after evaporation of the solvent. Identification of the TCA is achieved by constant neutral loss (CNL) scans for 173 u, 195 u and 193 u and subsequent daughter ion spectra of the molecular ions [M+H]+. Glucuronide conjugate metabolites of the tricyclic antidepressants1,2,3,6,8could be identified by CNL-scans (176 u) and the assignments were confirmed by daughter ion mass spectra. A urine sample of a fatal1,2,8overdose and samples of three patients under therapeutic dosage with1,3or6are presented as examples for application.

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A screening method for the rapid detection of barbiturates in serum by means of tandem mass spectrometry

Cited by 7 publications

References 8 publications

Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbital and thiopental in human serum

Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbital and thiopental in human serum

Investigation of corona discharge ionization of barbituric acid using ion mobility spectrometry along with quantum chemical calculations

A fast screening method for tricyclic antidepressants and their urinary metabolites by FAB‐tandem mass spectrometry

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