Gas Chromatography-Mass Spectrometry of Catecholamines and Tryptamines: Determination of Gas Chromatographic Profiles of the Amines, Their Precursors and Their Metabolites

Simultaneous quantification of dopamine, 5-hydroxytryptaine and four metabolically related compounds by means of reversed-phase high-performance liquid chromatography with electrochemical detection

“…A variety of separation and detection methods have been used to quantify the precursors and metabolites of dopamine and 5-HT. Of these techniques, the greatest degrees of flexibility, sensitivity and specificity have been obtained using either gas chromatography with electron-capture or mass fragmentographic detection [15][16][17][18][19][20][21], or high-performance liquid chromatography (HPLC) using fluorometric or electrochemical detection [22][23][24][25][26][27][28][29][30][31][32][33][34][35][36][37]. However, each of these techniques has potential shortcomings in at least one of the following criteria: speed; sensitivity; specificity; flexibility; sample purification and/or concentration; use of internal standards to monitor recovery during sample preparation; or complexity of instrumentation.…”

Analysis of acidic monoamine metabolites by gas chromatography-mass spectrometry

“…In this case the products were detected by double ion monitoring at 438 amu (M+ -COOCH2C2F6) for la and 469 with pentafluoropropionic anhydride-pentafluoro-n-propanol (Ila and lib), pentafluoropropionic anhydride-trifluoroethanol (lie and lid) and methanol-HCI followed by pentafluoropropionic anhydride (He and I If) to 3 h, as described by Gelpi et al (6), product la was formed almost quantitatively (Figure 3). Since there were two possible alternative structures for lb (i.e., where Rj = H and R2 = COC2F5 or Rx = COC2F5 and R2 = H) (Gelpi et al ( 6)), it was necessary to verify the proposed structure of lb as shown.…”

“…For acidic monoamine metabolites, prior methylation of the carboxyl moiety with ethereal diazomethane followed by acylation with pentafluoropropionic or heptafluorobutyric anhydride has provided suitable volatile derivatives for analysis (3,5). However, esterification of these metabolites using the above reagents may result in multiple products depending on the number of potential molecular sites of esterification and the reaction conditions employed (6,7). These multiple products may give reduced sensitivity and also may result in loss of specificity in the case of selective ion monitoring GC-MS or gas-chromatography (GC) with electron capture detection.…”

Untersuchungen zur Trifluoracetylierung der Methylderivate von Tryptamin und Serotonin mit verschiedenen Derivatisierungsreagentien: Synthesen, Spektroskopie sowie analytische Trennungen mittels Kapillar-GC / Trifluoroacetylation of Methylated -Derivatives of Tryptamine and Serotonine by Different Reagents: Synthesis, Spectroscopic Characterizations, and Separations by C apillary-Gas-Chromatography

“…D ie später angew andten g as-chrom atographi schen (G C ) T rennverfahren b en ü tzten zunächst gepackte Trennsäulen zur B estim m ung von 4 und 8 im U rin für: Trim ethylsilylderivate (TM S) m it tels: G C -FID : [23], GC-M S: [24,39]; für Trifluoracetylderivate (TFA ) m ittels G C -FID : [40], G C-MS: [41], G C-M S-PN D : [42][43][44], m ittels G C -E C D bei D erivatisierung m it H eptafluorbutyrylim idazol (H F B I) [45] oder nach D erivatisierung m it Pentafluorpropionylanhydrid (PFPA ) [46], D ab ei bietet allein die G C -M S-K om bination m it SIM oder M ID, z. B. nach H F B I-D erivatisierung [47], v er lässliche Ergebnisse.…”

“…Die oben erw ähnten L iteratu rb efu n d e [39][40][41][42][43][44][45][46] sind auch un ter A nw endung n eu er em pfindlicher und spezifischer D etektions-T echniken [52] wie z. B.: E C D = E lek tro n en ein fan g -D etek to r mit 63Ni, PN D = stickstoffspezifischer Flam m enionisations-D e te k to r o der m assenspektroskopische selektive D etek tio n durch: SIM = single ion m onitoring, M ID = m ultiple ion detection, nicht w iderspruchs frei, was w ahrscheinlich auf chemische Schwierig keiten bei d er Probenaufbereitungstechnik sowie vor allem bei den für die G C -U ntersuchungen ge w ählten D erivatisierungsreaktionen zurückzufüh ren ist.…”