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Lecture 23 Mass Spectroscopy III Harris Ch.22
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Nitrogen Rule Mass Number C 12 H 1 O 16 F 19 Cl 35 or 37 Br 79 or 81 I 127 S 32 Si 28 N 14 CH 4 16 C n H 2n+2 Even number Replace H by any group: OH, F, Cl, Br, I, SH, SiH 3 Still even number! Replace 2H by O, S, etc. Still even number! Any saturated hydrocarbon Replace by –NH 2 ODD! Mass number is odd: I have odd number of N atoms
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High resolution MS
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LSD
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A 1.0 g whole blood or 1.0 mL urine was mixed with 20 μL 0.05 mg/l aqueous LSD-D3. The sample was extracted with 1.0 mL butyl acetate after adjusting pH with 1.0 mL 1 M sodium carbonate. After centrifugation for 10 min at 3600 rpm, the organic fraction was removed and evaporated to dryness at 40 °C under a steam of pure nitrogen. It was reconstituted in 100 μL mobile phase and transferred to a brown autosampler vial and 20 μL was injected into the chromatographic system. LSD324 → 223324 → 2080.61 Iso-LSD324 → 281a324 → 2081.0 M-LSD356 → 237356 → 2220.84 IS (D3-LSD) 327 → 226––
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