Rapid determination of barbiturates by gas chromatography-mass spectrometry

Skinner, Ronald F.; Gallaher, E G.; Predmore, D. B.

doi:10.1021/ac60325a035

Cited by 36 publications

(4 citation statements)

References 10 publications

(7 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The mass spectra of the chromophore and DMBA are shown in Figure 3. According to the mass spectrum of DMBA and the previous papers reported by Gilbert et (21,22), the postulated fragmentation pattern is given in Figure 4. The results indicate as expected that the chromophore was produced from the reaction of DMBA and malonaldehyde (III, a tautomer of 3-hydroxy-2-propenal; eq 2) which derived from the cleavage of the pyrimidine ring.…”

Section: Discussionmentioning

confidence: 75%

Dicyclohexylcarbodiimide as a cleaving agent for colorimetric determination of pyridyl and pyrimidinyl compounds

Chen¹

1985

Anal. Chem.

View full text Add to dashboard Cite

1461were dispersed within each other with sufficient reproducibility that standard addition could be performed over a wide, controllable range of standard/analyte concentration ratios. I t is interesting to observe that the new variant of the gradient technique is partially based on the underlying concept of FIA titration ( I ) , where elements of fluid with identical D values are exploited, and partially on the concept of zone penetration (5) as designed for selectivity measurements, where elements of fluid with identical delay times t were used.Thus, another variation of the concept dispersed sample zone has been discovered and exploited. Its use is not limited to flame methods, as reaction based assays, like spectrophotometry, would equally benefit from the novel way of performing standard addition. Instruments equipped with photodiode arrays and appropriate fast data collection and storage facilities should increasingly find use in future applications.By use of dlcyclohexylcarbodAmIde (DCC) and dimethylbarblturic acid (DMBA) as reagents, a colorlmetric method for the deterrninatlon of pyrldyl and pyrlmldlnyl compounds has been established. DCC breaks the pyrldlne or pyrlmldine ring to afford giutaconaldehyde or maionaldehyde and then reacts wlth DMBA to produce chromophores. These heterocycles could be determined by measuring the chromophores. The reiatlve standard devlatlons obtained with different amounts of these compounds were In the range of 0.63 to 5.36% ( n

show abstract

Section: Discussionmentioning

confidence: 75%

Dicyclohexylcarbodiimide as a cleaving agent for colorimetric determination of pyridyl and pyrimidinyl compounds

Chen¹

1985

Anal. Chem.

View full text Add to dashboard Cite

show abstract

“…A summary of chromatographic methods developed to detect barbiturates in biological samples is shown in Table . Compared with other similar GC‐MS methods that used conventional sample preparation techniques (LLE or SPE) for the extraction of barbiturates , the present method uses much less solvent per sample and consequently less residues are generated. Simplicity, rapidity, and less sample manipulation are other advantages that can be seen over these methods.…”

Section: Resultsmentioning

confidence: 99%

Hollow‐fiber liquid‐phase microextraction and gas chromatography‐mass spectrometry of barbiturates in whole blood samples

Menck

Lima

Seulin

et al. 2012

J of Separation Science

View full text Add to dashboard Cite

Here, we present a method for measuring barbiturates (butalbital, secobarbital, pentobarbital, and phenobarbital) in whole blood samples. To accomplish these measurements, analytes were extracted by means of hollow-fiber liquid-phase microextraction in the three-phase mode. Hollow-fiber pores were filled with decanol, and a solution of sodium hydroxide (pH 13) was introduced into the lumen of the fiber (acceptor phase). The fiber was submersed in the acidified blood sample, and the system was subjected to an ultrasonic bath. After a 5 min extraction, the acceptor phase was withdrawn from the fiber and dried under a nitrogen stream. The residue was reconstituted with ethyl acetate and trimethylanilinium hydroxide. An aliquot of 1.0 μL of this solution was injected into the gas chromatograph/mass spectrometer, with the derivatization reaction occurring in the hot injector port (flash methylation). The method proved to be simple and rapid, and only a small amount of organic solvent (decanol) was needed for extraction. The detection limit was 0.5 μg/mL for all the analyzed barbiturates. The calibration curves were linear over the specified range (1.0 to 10.0 μg/mL). This method was successfully applied to postmortem samples (heart blood and femoral blood) collected from three deceased persons previously exposed to barbiturates.

show abstract

“…The solvent was removed and the milky viscous liquid was purified by column chromatography using silica gel (0.05-2 mm) with methylene chloride as elution solvent to give Metabolite 4, mp 83O, in 40% yield. The loss of ethyl isocyanate, C2H5CNO (242 -171 or 227 -156) supported by metastable peaks m* in the final sequence is characteristic of uracil and barbituric acid derivatives in a retro-Diels-Alder fragmentation (6)(7)(8). The fragmentation of I can be formulated according to Scheme I.…”

mentioning

confidence: 99%

2- 14C-1 -Allyl-3,5-diethyl-6-chlorouracil II: Isolation and Structures of the Major Sulfur-Free and Three Minor Sulfur-Containing Metabolites and Mechanism of Biotransformation

Kaul

Hempel

Kiefer

1982

Journal of Pharmaceutical Sciences

View full text Add to dashboard Cite

Rapid determination of barbiturates by gas chromatography-mass spectrometry

Cited by 36 publications

References 10 publications

Dicyclohexylcarbodiimide as a cleaving agent for colorimetric determination of pyridyl and pyrimidinyl compounds

Dicyclohexylcarbodiimide as a cleaving agent for colorimetric determination of pyridyl and pyrimidinyl compounds

Hollow‐fiber liquid‐phase microextraction and gas chromatography‐mass spectrometry of barbiturates in whole blood samples

2- 14C-1 -Allyl-3,5-diethyl-6-chlorouracil II: Isolation and Structures of the Major Sulfur-Free and Three Minor Sulfur-Containing Metabolites and Mechanism of Biotransformation

Contact Info

Product

Resources

About