Mass Spectroscopy III

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Lecture 23

• Mass Spectroscopy III
• Harris Ch.22

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Nitrogen Rule
Mass number is odd I have odd number
of N atoms
Mass Number
CH4
16
C 12 H 1 O 16 F
19 Cl 35 or 37 Br 79 or 81 I
127 S 32 Si 28 N
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Any saturated hydrocarbon
CnH2n2
Even number
Replace H by any group OH, F, Cl, Br, I, SH,
SiH3
Still even number!
Replace 2H by O, S, etc.
Still even number!
ODD!
Replace by NH2
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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.
LSD 324 ? 223 324 ? 208 0.61 Iso-LSD 324 ?
281a 324 ? 208 1.0 M-LSD 356 ? 237 356 ?
222 0.84 IS (D3-LSD) 327 ? 226
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