Modifications papar and thin layer chromatographic methods to increase sensitivity for detecting N-methylated indoleamines in urine.

A critical review of reports of endogenous psychedelic N, N‐dimethyltryptamines in humans: 1955–2010

“…Gjessing [13] HDMT TLC (2-D), color reaction ND Rf and color (2-D) 1965 Takesada et al [14] HDMT paper chromatography, color reaction [15] HDMT paper chromatography, color reaction ND Rf and color (2-D) 1966 Perry et al [16] DMT, HDMT paper chromatography (2-D), color reaction 2 mg/24 hr for DMT and HDMT Rf and color (2-D) 1966 Heller [17] HDMT paper chromatography (2-D), color reaction ND Rf and color (2-D) 1967 Fischer and Spatz [18] HDMT paper chromatography (2-D), color reaction ND Rf and color (2-D) 1967 Kakimoto et al [19] DMT, HDMT paper chromatography (3 systems), color reaction 10 mg/24 hour Rf and color (3 systems) 1967 Tanimukai [20] HNMT, HDMT, NMT, DMT, paper and TLC (2-D); color reaction; GC-FID of HDMT 5 ng/ml HDMT; 1 ng/ml others Rf and color (2-D paper, TLC) MDMT 1967 Tanimukai et al [21] HDMT paper chromatography, TLC (2-D), color reaction; GC-FID >0.1 mg/24 hour Rf and color (2-D); GC-RT 1967 Tanimukai et al [22] HDMT paper and TLC (2-D); color reaction; GC-FID of HDMT ND Rf and color (2-D paper, TLC); GC-RT 1967 Acebal and Spatz [23] HDMT paper chromatography (2-D), color reaction ND Rf and color (2-D) 1968 Faurbye and Pind [24] HDMT paper chromatography and TLC, color reaction >0.7 mg/24 hour Rf and color (paper and 2-D TLC) 1969 Sireix and Marini [25] HDMT UV; paper chromatography, color reaction ND Rf and color (2-D) 1969 Spatz et al [26] HDMT UV of diazo-deriv; paper chromatography, color reaction ND UV; Rf and color 1970 Fischer and Spatz [27] HDMT UV; TLC, color reaction ND UV; Rf and color 1970 Saavedra and Udabe [28] HDMT UV; TLC, color reaction ND UV; Rf and color 1970 Tanimukai et al [29] HNMT, HDMT, DMT, MDMT paper and TLC (2-D); color reaction; GC-FID of HDMT ND Rf and color (2-D paper, TLC); GC-RT 1970 Heller et al [30] DMT, MDMT, HDMT GC-FID, TLC, and Spectrofluorometry 2 ng/ml GC-RT and TLC or spectrofluorometer 1971 Narsimhachari et al [31] DMT, MDMT, HDMT TLC and GC-FID, verified with spectrofluorometer 5 mg/ml per 24hour for DMT TLC and GC-FID, spectrofluorometer 1971 Narasimhachari et al …”

“…Thus, a total of 40 individuals were positive (29%) and 96 were negative. [20] Although there do not seem to be any published replications of Tanimukai's findings, they did lead to modification of many of the extraction procedures that were subsequently designed to fractionate tertiary from primary amines ( Table 1). [60] The above does not address the analytical methods' sensitivity and specificity, and assumes that all of the data as collected and reported are accurate, either in their detection or non-detection of the target analyte(s) or the concentrations observed.…”

“…[85] Early criticisms of reports of endogenous psychedelics were directed at the fact that rather non-specific chemical tests were being applied, double-blind analyses were not always being performed, and dietary or medication sources were not always adequately ruled out as responsible for the identifications. [2,12] Further, it was claimed that possible artifacts produced from the extraction solvents and conditions of analysis may have led to misidentification of the DMTs in some early studies [20] and, more recently, that the use of halogenated solvents in the analysis may have affected their detection. [86] Biological factors that may have affected the detectabilty of these compounds in the periphery were also acknowledged, which included their rapid metabolism.…”

“…Takesada et al [14] HDMT 24 hour urine Ext, Dowex 50 column, alumina column 1966 Runge et al [15] HDMT 1 L of urine pH 8-9, butanol ext, acetone ppt, acetone 1966 Perry et al [16] DMT, HDMT Heller [17] HDMT 1 L of urine NaHCO3 sat., butanol, evap, acetone 1967 Fischer and Spatz [18] HDMT 100 ml fresh urine NaCO3, ether ext, evap, acetone 1967 Kakimoto et al [19] DMT, HDMT 24 hour urine; vol 600 mg creatinine analyzed Ext, Dowex 50 column, alumina column 1967 Tanimukai [20] HNMT, HDMT, NMT, DMT, MDMT Fischer et al [33] HDMT, glucuronide 50 ml morning urine; w/wo glucuronidase Liquid-Liquid ext; w/wo glucuronidase treatment 1972 Himwich et al [34] HDMT, DMT, MDMT Narasimhachari et al [35] HDMT, DMT, MDMT 24 hour urine Walker et al [36] DMT plasma; DMT stable for 60 days at 6 degrees C HCL ext acid pH with CHCl3, pH 9, ext CHCl3, evap Wyatt et al [37] DMT plasma HCL ext acid pH with CHCl3, pH 9, ext CHCl3, evap 1973 Narasimhachari and Himwich [38] DMT, HDMT Lipinski et al [39] DMT plasma separated by centrifugation HCL ext acid pH with CHCl3, pH 9, ext CHCl3, evap 1974 Bidder et al [40] DMT Heparinised plasma or whole blood; 24 hr urine HCL ext acid pH with CHCl3, pH 9, ext CHCl3, evap 1974 Narasimhachari et al [41] HDMT, DMT, MDMT Forsstrom et al [67] DMT, MDMT, HDMT, NMT morning and afternoon urines; 5 ml assayed urine centrifuged and ext on Oasis SPE cartridge 2005 Karkkainen et al [68] DMT, HDMT urine (5 ml), plasma or serum (1 ml), stool;…”

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

“…B. U rin w aren, trotz selektiver A n färbung durch S prühreagentien, viel zu wenig em pfindlich und kaum substanzspezifisch [28][29][30] und führten dah er auch zu w idersprüchlichen E r gebnissen: positiv: [27,28,[31][32][33][34][35] und negativ: [36 -38]. Die D C wird heute nur noch p räp arativ zur analytischen V ortrennung d er U rin p ro b e n b e nützt.…”