Liquid Chromatography-Mass Spectrometric Analysis of Tropane Alkaloids in Mammalian Samples: Techniques and Applications - LC-MS in Drug Bioanalysis - page 316

Table 7 Tropane alkaloid analysis by LC-MS and LC-MS/MS for biotransformation studies in vivo and in vitro

Column (mm × mm)/ fl ow (ml/min)/ T
(°C)

Ionization/mass
analyser/scan mode Reference Analyte Mobile phase a (run mode) Lin range (ng/ml) b

Ada c AICHROM ReliAsil C18

(150 × 2)/0.2/40

MeOH/0.01 % Et 3 N, pH 3.5, 60:40 (iso) n.s. ±ESI/IT/MS/MS [ 6 ]

Adi c AICHROM ReliAsil C18

(150 × 2)/0.2/40

MeOH/0.01 % Et 3 N, pH 3.5, 60:40 (iso) n.s. ±ESI/IT/MS/MS [ 5 ]

Atr c Zorbax extend C18 (100 × 3)/0.2/40 MeOH/2 mM NH 4 OAc, pH 3.5 70:30 (iso) n.s. +ESI/IT/MS/MS [ 51, 52 ]

Beme d Spherisorb CN (250 × 4.6) or Spherex

C-18 (250 × 4.6)/1.0/n.s.

Solv A: 0.05 M NH 4 OAc, pH 4.4
Solv B: 0.05 M NH 4 OAc/ACN 55:45
Solv C: 0.05 M NH 4 OAc/ACN 40:60 (gradient)

n.s. +TSP/SQ/n.s. [ 37 ]

Benz e CSC spherisorb cyano

(100 × 25)/0.006 j /n.s.

H 2 O/ACN 80:20, 0.1 % HOAc (iso) n.s. +ESI/SQ/MS [ 59 ]

Cim f Spherisorb ODS-2 (250 × 4.6)/1.0/n.s. 20 or 35 mM hep-SA, 100 mM Et 3 N in MeOH/

ACN/H 2 O 20:20:55 or 5:10:55 , pH 3.7 (iso)

30-150 +FAB (Xe)/EBQ 1 Q 2 /

MS/MS

[ 23, 62 ]

Scp g Zorbax extend C18 (100 × 3)/0.2/40 MeOH/2 mM NH 4 OAc, pH 3.5 70:30 (iso) n.s. +ESI/IT/MS/MS [ 7, 87 ]

Trop h Nucleosil C4 (250 × 4.6)/0.5/35 Solv A: ACN/20 mM NH 4 OAc 10:90, pH 6.0

Solv B: ACN/20 mM NH 4 OAc 60:40, pH 6.0
(gradient)

70-1,425 +ESI/SQ/SIM [ 82 ]

Atr, BuS, Coc,
Hatr, Ipra,
Lit, Scp i

Atlantis T3 C18 (150 × 4.6)/1.0/30 Solv A: 0.1 % v/v FA

Solv B: ACN/0.1 % FA 80:20 v/v (gradient)

Atr, Coc, Ipra, Lit,
Scp: 0.05-50
Hatr: 0.1-50
BuS: 0.8-50

+ESI/QqQ/MRM [ 50 ]

R -/ S -Hyo i AGP (2x 150 × 2)/0.3/40 Solv A: 10 mM NH 4 FA, pH 8.0

Solv B: 10 mM NH 4 FA in 25 % ACN, pH 8.0;
85:15 (iso)

1-500 +ESI/QqQ/MRM [ 49 ]