Drug Metabolism in Drug Design and Development Basic Concepts and Practice

TABLE 3.6 Examples of LC/MS assays employed to study sulfonate conjugates.Substrate

LC/MS assay details

Ion

References

Curcuminoids

System: LC–MS on a PE Mariner MS system

[M

+H]

+: Curcumin

m

/z

= 369.13

curcumin sulfate

m

/z

= 449.09

Asai and Miyazawa (2000)

LC: TSKgel-ODS 80Ts column, 40

C; 5% folic

acid, 5 mM ammonium acetate in acetonitrile(ACN): water 50 : 50 v/v at 1 mL/min

MS detection: ES, positive mode

Quercetin

System: LC/MS on a Finnigan

MAT 95 system

Quercetin

m

/z

301

van der Woude et al. (2004)

LC: C18 5 U column; 0.1% acetic acid

in 20–80% ACN over 30 min at0.2 mL/min

Monosulfate

m/

z^381

MS detection: ES, negative mode,

source 4.5 kV, capillary 180

C

Genistein

System: LC/MS/MS on a PE series

200 HPLC system with PE SciexAPI 3000 triple quadrupole MS,ESI interface

Genistein

m/

z

269.3–133.1

Soucy et al. (2005)

LC: C18 column; 5 mM ammonium

acetate pH 7.0 and ACN 5–95%over 11 min at 0.2 mL/min

Genistein sulfate

m/

z349.2–269.3

MS detection: MRM, negative modeIS: chrysin

p-OH-methamphetamine

(pOHMA)

(Metabolite identification) System:

LC/MS/MS on a ShimadzuLCMS-IT-TOFsystem, ESI interface

pOHMA

m

/z

166

Shima et al. (2005)

LC: L-column ODs semi-micro; 10 mM

ammonium formate pH 3.5: methanol(95 : 5 v/v)

pOHMA-sulfate

m/

z^246

MS detection: ESI, positive mode,

source 4.5 kV, capillary 200

C

70