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Christie J, White MW, Wiles JM. 
“A chromatographic method for the detection of LSD in biological 1iquids”. 
J.Chromatog.. 1976;120(2):496-501.
The detection of LSD in human biological fluids by a combination of HPLC and TLC is reported. Urine, adjusted to pH3 with HC1, was extracted 3x with Et2O the aqueous layer was basified to pH9 with NH3 and then reextracted. The sample was evaporated and the residue was taken up in the mobile phase of MeOH-H2O-NllNO3 before injection onto an HPLC column packed with partisil (average size of particle = 6 Urn) with a mobile phase flow-rate of 1 ml/min and pressure of 2000 psi; a fluorescence detector was employed (Iex=355, em=430 nary). Two fractions were obtained and the first was -eated with AcOH then NaHCO3, extracted with CH2C12 then subjected to TLC on silica gel FZ54. The other fraction was treated analogously with the omission of AcOH. Fatty deposits were removed by elusion with CHzClz then developers (Me)2COCHCl3-MeOH 15:4:1 and 4 its respectively were used for LSD (fraction 1) and iso-LSD (fraction 2). The spots were detected with UV and p-dimethylaminobenzaldebyde, extracted from the plates, treated with tartaric acid/MeOH and confirmed by MS. Analysis of a sample of LSD-tartrate indicated that some isomerization of LSD to iso-LSD occurred during the process. The extraction procedure was 70 0.000000e+00fficient. The method was applied to urine, blood, plasma and bile samples of people who had taken LSD and a range of 0.3-19.5 ng/nl were isolated.
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