Trimethylsilyl Derivatization and Gas Chromatograph–Mass Spectrometric Determination of Aspirin and Its Major Metabolites, I

Mongillo, J.A.; Paul, J.

doi:10.1006/mchj.1996.1301

Cited by 2 publications

(4 citation statements)

References 8 publications

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“…26,27 As a result, like many other pharmaceutical agents, it cannot be directly analyzed by conventional GC, since it is destroyed when subjected to the high-temperature conditions of the injector and oven. 28 Accordingly, ASA must be derivatized by lengthy procedures to analyze it by conventional GC, 13,[29][30][31] and it is normally analyzed by HPLC instead. 32 Therefore, it was another interesting sample to analyze with the ultrashort GC column setup.…”

Section: System Operating Characteristicsmentioning

confidence: 99%

A novel ultrashort capillary gas chromatography method using on-column injection and detection

2016

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A novel method for ultrashort capillary column gas chromatography (GC) analysis is introduced, which employs on-column injection and detection and rapid temperature programming. Using 10-20 cm long capillary columns, results showed that the method provides efficient and very rapid separations for relatively simple mixtures. Moreover, the on-column aspect of the method used here is demonstrated to avoid the extra column analyte degradation that can occur in traditional approaches to such separations. As a result, the developed method allows for the first time the GC analysis of some very large and (or) highly thermally labile analytes, such as polypeptides and drug molecules that are normally prone to decomposition. As an application, this method is further used to monitor pharmaceutical degradant formation as a function of temperature and was found to provide similar results to those obtained from conventional high-performance liquid chromatography analysis. Overall, the findings indicate that this ultrashort GC column approach could be useful in these areas and potentially others, where relatively simple GC analysis and universal flame ionization detection is desirable.Key words: ultrashort column, gas chromatography, flame ionization detection, on-column injection, rapid heating.Résumé : Nous présentons une nouvelle méthode d'analyse par chromatographie en phase gazeuse (CPG) sur colonne capillaire ultracourte, dans laquelle est employé un système d'injection et détection sur colonne et un réglage de chauffage rapide. Avec des colonnes capillaires de longueurs allant de 10 à 20 cm, les résultats indiquent que la méthode permet des séparations efficaces et très rapides de mélanges relativement simples. En outre, nous avons démontré que l'aspect « sur colonne » de la méthode dont il est question permet de limiter la dégradation des analytes dans la colonne, qui peut se produire au cours de ce type de séparation par les méthodes classiques. Par conséquent, la méthode mise au point permet de réaliser pour la première fois l'analyse par CPG de certains analytes très volumineux ou très thermolabiles comme les polypeptides et les molécules thérapeutiques normalement sujettes à la décomposition. En ce qui concerne son application, la méthode peut également être utilisée pour surveiller la formation des produits de dégradation pharmaceutiques en fonction de la température et se révèle utile pour produire des résultats similaires à ceux qui sont obtenus par l'analyse conventionnelle par chromatographie en phase liquide à haute performance. En conclusion, les résultats indiquent que cette méthode employant une colonne de CPG ultracourte peut être utile dans ces domaines, et éventuellement dans d'autres domaines où une analyse par CPG relativement simple avec une détection à ionisation de flamme est souhaitable. [Traduit par la Rédaction] Mots-clés : colonne ultracourte, chromatographie en phase gazeuse, détection à ionisation de flamme, injection sur colonne, chauffage rapide.

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Section: System Operating Characteristicsmentioning

confidence: 99%

A novel ultrashort capillary gas chromatography method using on-column injection and detection

2016

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“…The dried residues were each derivatized by treating with 200 mL of BSTFA and heating at 90ЊC for 1 h on a Reactitherm heating system. The derivatization procedure is performed in accordance with Part I of this publication (1). The final concentrations in this solution were 100 mg/mL for each of the five compounds.…”

Section: Recovery and Matrix Effectsmentioning

confidence: 99%

“…It is easily hydrolyzed to salicylic acid, which, in turn, is metabolized to free and conjugated forms of other compounds (1)(2)(3). Some of the compounds present in human urine following its metabolism include salicylic acid, gentisic acid, and salicyluric acid.…”

Section: Introductionmentioning

confidence: 99%

“…The extraction is tested for recovery using authentic materials spiked into a control urinary matrix and yields excellent recovery and reproducibility for all metabolites. The derivatization procedure fully derivatized each species without any detected reaction degradation (1,4,5). These samples, still in the derivatizing agent, were injected neat into the GC/MS system.…”

Section: Introductionmentioning

confidence: 99%

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Determination of Aspirin and Its Major Metabolites in Human Urine by Gas Chromatography–Mass Spectrometry, II

Mongillo

Paul

1997

Microchemical Journal

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Trimethylsilyl Derivatization and Gas Chromatograph–Mass Spectrometric Determination of Aspirin and Its Major Metabolites, I

Cited by 2 publications

References 8 publications

A novel ultrashort capillary gas chromatography method using on-column injection and detection

A novel ultrashort capillary gas chromatography method using on-column injection and detection

Determination of Aspirin and Its Major Metabolites in Human Urine by Gas Chromatography–Mass Spectrometry, II

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