Basic drug analysis by strong cation-exchange liquid chromatography-tandem mass spectrometry: simultaneous analysis of amisulpride, and of metamfetamine and amfetamine in serum/plasma

TY - JOUR

T1 - Basic drug analysis by strong cation-exchange liquid chromatography-tandem mass spectrometry

T2 - simultaneous analysis of amisulpride, and of metamfetamine and amfetamine in serum/plasma

AU - Couchman, Lewis

AU - Morgan, P. E.

AU - Flanagan, Bob

PY - 2011/8

Y1 - 2011/8

N2 - In the HPLC of basic drugs and metabolites, good efficiency and peak shape can often be attained using strong cation-exchange packings with isocratic 100% methanol eluents containing an ionic modifier at an appropriate pH* and ionic strength. Solvent extracts can be analysed directly, and use of ammonium acetate as modifier facilitates the use of atmospheric pressure chemical ionization (APCI)-tandem mass spectrometry, selected reaction monitoring mode. For the analysis of amisulpride and of metamfetamine/amfetamine in plasma (200 mu L) after single oral doses in man, a column packed with Waters Spherisorb S5SCX (5 mu m average particle size, 100 2.1 mm i.d.) was used with methanolic ammonium acetate (40 mmol/L, pH* 6.0, flow rate 0.5 mL/min) as eluent (35 degrees C). Deuterated internal standards were used for each analyte. Detection was by positive-mode APCI. Responses for all analytes were linear over the calibration ranges. Intra-assay precision (RSD) was 2-18%, and inter-assay precision was 2-12%. The limit of detection was 0.5 mu g/L for all analytes. No significant matrix effects or isobaric interferences were noted. The total analysis time was 7 min. Similar methodology can be applied to a wide range of basic analytes using MS/MS detection.

AB - In the HPLC of basic drugs and metabolites, good efficiency and peak shape can often be attained using strong cation-exchange packings with isocratic 100% methanol eluents containing an ionic modifier at an appropriate pH* and ionic strength. Solvent extracts can be analysed directly, and use of ammonium acetate as modifier facilitates the use of atmospheric pressure chemical ionization (APCI)-tandem mass spectrometry, selected reaction monitoring mode. For the analysis of amisulpride and of metamfetamine/amfetamine in plasma (200 mu L) after single oral doses in man, a column packed with Waters Spherisorb S5SCX (5 mu m average particle size, 100 2.1 mm i.d.) was used with methanolic ammonium acetate (40 mmol/L, pH* 6.0, flow rate 0.5 mL/min) as eluent (35 degrees C). Deuterated internal standards were used for each analyte. Detection was by positive-mode APCI. Responses for all analytes were linear over the calibration ranges. Intra-assay precision (RSD) was 2-18%, and inter-assay precision was 2-12%. The limit of detection was 0.5 mu g/L for all analytes. No significant matrix effects or isobaric interferences were noted. The total analysis time was 7 min. Similar methodology can be applied to a wide range of basic analytes using MS/MS detection.

KW - HPLC-MS/MS basic drugs

KW - HPLC-MS/MS amfetamine/metamfetamine

KW - HPLC-MS/MS amisulpride

KW - HPLC

KW - ELUENTS

U2 - 10.1002/bmc.1530

DO - 10.1002/bmc.1530

M3 - Article

SN - 0269-3879

VL - 25

SP - 867

EP - 872

JO - Biomedical Chromatography

JF - Biomedical Chromatography

IS - 8

ER -