The development of a method is described for the analysis of hydroxypipecolic acids in crudely purified plant extracts. All eight known naturally-occurring mono-and di-hydroxypipecolic acids could be resolved in a single analysis by gas chromatography-mass spectrometry (GC-MS) of their trimethylsily
Derivatization methodology for the analysis of butorphanol by gas chromatography-mass spectrometry
β Scribed by Maristela Haddad Andraus; Maria Elisa Pereira Bastos de Siqueira
- Publisher
- John Wiley and Sons
- Year
- 1998
- Tongue
- English
- Weight
- 81 KB
- Volume
- 12
- Category
- Article
- ISSN
- 0269-3879
No coin nor oath required. For personal study only.
β¦ Synopsis
Butorphanol is an opioid used as analgesic in humans and other species. In horses, it can cause locomotor stimulation at low doses. This drug is not well chromatographed by GC and so, it is necessary to transform it into a more suitable compound, which can be done by derivatization. The derivatization of a drug is used to impart volatility, masking polar groups to improve the results in gas chromatographic analysis. We have evaluated N,Obis(trimethylsilyl)-trifluoracetamide (BSTFA) + 1% trimethylchlorsilane (TMCS) and N-methyl-N-trimethylsililtrifluoroacetamide (MSTFA) as derivatizing reagents for butorphanol at 30, 60 and 80ΨC during 15, 30 and 60 min. The effects of dilution of these reagents with toluene and the evaporation before the derivatization were tested. Both reagents can be used for butorphanol derivatization and analysis and the dilution and evaporation steps did not alter the final results. The best derivatization conditions were 15 min at 80ΨC, although 60ΨC, although 60ΨC during 60 min were also suitable.
π SIMILAR VOLUMES
The analysis of peptide derivatives by fast atom bombardment, liquid secondary-ionization mass spectrometry, plasma desorption, electrospray ionization, and matrix-assisted laser desorption/ionization is reviewed. The fragmentation patterns of peptides and of charge-derivatized peptides are compared
A novel chemical ionization/fast atom bombardment (CI/FAB) source was used to analyse alkenes by chemical ionization mass spectrometry (CI-MS) using copper ions as the ionizing agent. The Cu Y -CI mass spectra showed abundant pseudomolecular adduct ions [alkene-Cu] Y and characteristic fragment ions
The technique developed by Husek and modified by this laboratory for the derivatization of amino acids in aqueous solution using ethylchloroformate/trifluoroethanol/pyridine prior to gas chromatography positive-and negative-ion chemical ionization mass spectrometry was extended to the analysis of a
A method was developed for the analysis and characterization of quercetin and kaempferol in urine following ingestion of Ginkgo biloba tablets. The method utilized gas chromatography/negative ion chemical ionization mass spectrometry of the trimethysilyl derivatives of the flavonoids. Limits of dete