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16/12/2018 18:01

Applicazione della settimana

Analisi di conferma di cannabinoidi in LC/MS/MS

Analisi di conferma di cannabinoidi in LC/MS/MS

Utilizzando colonne Allure® Biphenyl

Utilizzando le colonne Allure® Biphenyl con HPLC Shimadzu Prominence e detector API MS/MS 3200 è possibile quantificare fino a 1ng di cannabinoidi non derivatizzati e separare ?9-THC e cannabidiolo alla linea di base in meno di 5 minuti. L'intensa interazione p-p incrementa notevolmente ritenzione e selettività della colonna bifenilica rispetto alle fasi C18. Utilizzando colonne Allure® Biphenyl ed un'interfaccaia elettrospray è possibile incrementare la % di metanolo incrementando la sensibilità. | Continua...

Table 1  MRM transitions for THC and metabolites: multiple transitions are monitored for each compound for definitive identifications.
Analyte
Q1 Mass
Q3 Mass
Time (ms)
DP (V)
EP (V)
CE (V)
CXP (V)
Hydroxy-THC (MRM1)
331.2
313.1
100
36
5
21
10
Hydroxy-THC (MRM2)
331.2
193.1
100
36
5
35
6
Carboxy-THC (MRM1)
345.2
327.0
100
41
4.5
21
10
Carboxy-THC (MRM2)
345.2
299.3
100
41
4.5
25
6
Cannabidiol (MRM1)*
315.2
193.2
100
36
4.5
31
6
Cannabidiol (MRM2)*
315.2
123.2
100
36
4.5
43
6
Cannabinol (MRM1)
311.2
223.0
100
46
8.5
27
8
Cannabinol (MRM2)
311.2
222.5
100
46
8.5
37
10
?9-THC (MRM1)*
315.2
193.2
100
41
4.5
33
6
?9-THC (MRM2)*
315.2
123.1
100
41
4.5
43
6
?9-THC-d3 (MRM1)
318.3
196.3
100
36
4.5
31
6
?9-THC-d3 (MRM2)
318.3
123.2
100
36
4.5
43
6
*Note, cannabidiol and ?9-THC share the same transitions, but are separated chromatographically.
DP — declustering potential, EP — entrance potential, CE — collision energy, CXP — collision cell exit potential

Final product spectra used in developing MRM transitions for compound identification and optimized sensitivity.

?9-THC

Carboxy-THC

Fast, selective separation of ?9-THC and its metabolites, using an Allure® Biphenyl HPLC column (extracted ion chromatography).

  1. 11-hydroxy-?9-tetrahydrocannabinol
  2. cannabidiol
  3. 11-nor-9-carboxy-?9-tetrahydrocannabinol
  4. cannabinol
  5. ?9-tetrahydrocannabinol
  6. ?9-tetrahydrocannabinol-d3

 

Sample:
Inj.:
10µL
Conc.:
100ng/mL each component
Sample diluent:
mobile phase
Column:
Allure® Biphenyl
Cat. #:
Dimensions:
30 x 2.1 mm
Particle size:
3µm
Pore size:
60Å
Conditions:
Instrument:
Shimadzu Prominence HPLC
Mobile phase:
A: 0.1% formic acid in water
B: 0.1% formic acid in methanol
Time (min.)
%B
0.5
2.5
5.0
6.0
6.1
50
90
90
50
Flow:
0.5mL/min.
Temp.:
ambient
Det.:
Spectrum Model (Sciex API 3200 Triple Quadrupole)
Interface:
ESI
Ion mode:
positive
Temp.:
500°C
Ion source:
5500V













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