The (M-43)+ Ion in the Mass Spectra of Some Medicinal Barbiturates

Coutts, Ronald T.; Locock, R.A.

doi:10.1002/jps.2600580635

Journal of Pharmaceutical Sciences

1969

DOI: 10.1002/jps.2600580635

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The (M-43)+ Ion in the Mass Spectra of Some Medicinal Barbiturates

Ronald T. Coutts

R.A. Locock

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1970

1993

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Cited by 12 publications

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“…In analyses by mass spectrometry (MS), sample extracts or the pure compounds can be introduced directly, thus avoiding derivatization and other problems associated with GC columns and detectors. Different ionization sources have been employed: El (38,39), Cl (40,41), FI (42), FD (42), and API (43). The El mass spectra of barbiturates do not always show molecular ions but the Cl spectra show the presence of protonated molecular ions from which the molecular weight can be determined.…”

mentioning

confidence: 99%

Identification of barbiturates by chemical ionization and mass-analyzed ion kinetic energy spectrometry

Soltero-Rigau¹,

Kruger²,

Cooks³

1977

Anal. Chem.

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routinely to ensure no contamination. Second, simultaneous quantitative multielement analysis of potassium through strontium is achieved in an irradiation time of 10-20 minutes. The analysis is nondestructive, so that the sample may be used to determine concentration of other elements, which are not determined by this method. Finally, the type of instrumentation used, lends the method to routine analyses (e.g., quality, control type analysis), on the order of 3 to 4 per hour. Thus, the analysis of various pharmaceuticals or analysis of repetitive environmental samples (i.e., sediment, plants, fish) can be greatly simplified.

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mentioning

confidence: 99%

Identification of barbiturates by chemical ionization and mass-analyzed ion kinetic energy spectrometry

Soltero-Rigau¹,

Kruger²,

Cooks³

1977

Anal. Chem.

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

Brzezinka¹,

Bold²,

Budzikiewicz³

1993

Biol. Mass Spectrom.

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A mass spectrometric screening method for barbiturates in serum was developed. Under electron impact conditions barbiturates fragment by loss of HNCO. A 'constant neutral loss' scan of 43 u provides, therefore, an indication of the presence of members of this toxicologically relevant class of compounds. Subsequent identification is possible either by 'daughter' or by 'parent ion' scans. The detection limit for propallylonal, buto- and phenobarbital was determined as better than 1 micrograms ml-1 serum.

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Reaktionen von 1,4‐Pentadien‐3‐onen, 12. Synthese und Struktur von 7,11‐Diphenyl‐2,4‐diazaspiro[5.5]‐undecan‐1,3,5,9‐tetraonen, I

Otto

Triepel

1976

Justus Liebigs Ann. Chem.

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Bei der Reaktion von I ,5-Diphenyl-l,4-peiitadien-3-on (2) mit an C-5 uimrhstituierten Barbitursauren 1 entstehen mit und ohne Basenkatalyse die Titelverbindungen 3. Dabei auftrctende Isomerengemische werdcn durch fraktionierende Kristallisation getrennt und die Strukturen mit spektroskopischen Methoden untersucht. Ein moglicher Mechanismus der Isonierisierung sowie eine Erklarung der Stereoselektivitat der Synthese werden diskutiert.Reactions of 1 ,.l-Pentadien-J-ones, 12 1). -Synthesis and Structure of 7,l l-Diphenyl-2,4-diazaspiro[5.5lundecane-l,3,5,9-tetraones, 1The title compounds 3 are synthesised from 1,5-diphenyl-1,4-pentadien-3-one (2) and barbituric acids 1, unsubstituted at C-5, with or without a basic catalyst. Isomers obtained are separated by fractional crystallization and the structures are elucidated by spectroscopic methods. A possible mechanism of isomerization and an explanation for stereoselectivity of t h e synthesis are discussed.Die basenkatalysierte Addition von aktivierten Methylengruppenz. €3. in Malonestern 2a), Phenylacetonitrilen 2b) und anderenan Pentadien-3-one fiihrt in der Regel zu Cyclohexanderivaten. Im Rahmen dieser Untersuchungen erschien es uns interessant, festzustellen, o b auch Methylengruppen in heterocyclischen Systemen, wie der Barbitursaure 1, an das Pentadienonsystem addiert werden konnen, und welche Strukturen die bei doppelter Addition zu erwartenden Spirane besitzen. Uber die Ergebnisse sol1 in dieser und der folgenden3) Mitteilung berichtet werden. SynthesenDie Barbitursiiuren l a -l f werden in alkoholischer Losung niit iiquimolaren Mengen 1,5-Diphenyl-l,4-pentadien-3-on (2) in Gegenwart basischer Katalysatoren wie NaOH, NaOR oder Aminen umgesetzt. Als bestes Verfahren hat sich die Reaktion mit Alkoholat in der Siedehitze bewahrt, obwohl auch hierbei, wie in allen anderen Fallen, harzige Nebenprodukte entstehen, die Z u n i Teil nur schwer abtrennbar sind und zu einer deutlichen Ausbeuteminderung fiiliren. Auch die Verwendung von *) Korrespondenz bitte an diesen Autor richten. 1 ) 11. Mitteilung: H.-H. Otto und U. Ebner, Arch. Pharm. (Weinhelm), im Druck. 2) 2a) H.-H. Orto, Monatsh. Chem. 104,526 (1973). -2b) U . Ebner und H.-H. Orto, Monatsh. Chem. 106, 601 (1975). 3) J . Triepel und H.-H. Otto, Veroffentlichung in Vorbereitung.

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The (M-43)+ Ion in the Mass Spectra of Some Medicinal Barbiturates

Cited by 12 publications

References 5 publications

Identification of barbiturates by chemical ionization and mass-analyzed ion kinetic energy spectrometry

Identification of barbiturates by chemical ionization and mass-analyzed ion kinetic energy spectrometry

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

Reaktionen von 1,4‐Pentadien‐3‐onen, 12. Synthese und Struktur von 7,11‐Diphenyl‐2,4‐diazaspiro[5.5]‐undecan‐1,3,5,9‐tetraonen, I

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