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A sensitive and selective method for the quantitative analysis of miglitol in rat plasma using unique solid‐phase extraction coupled with liquid chromatography–tandem mass spectrometry
Author(s) -
MizunoYasuhira Akiko,
Kinoshita Kohnosuke,
Jingu Shigeji,
Yamaguchi Junichi
Publication year - 2014
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.3185
Subject(s) - chemistry , chromatography , protein precipitation , solid phase extraction , electrospray ionization , tandem mass spectrometry , mass spectrometry , analytical chemistry (journal) , selected reaction monitoring , detection limit , extraction (chemistry) , liquid chromatography–mass spectrometry
A sensitive, selective and robust liquid chromatography–tandem mass spectrometry (LC‐MS/MS) method was developed for the quantification of miglitol in rat plasma. The sample preparation procedures involved protein precipitation and unique solid‐phase extraction, which efficiently removed sources of ion suppression and column degradation interference present in the plasma. Chromatographic separation was achieved on an amide column using 10 mmol/L CH 3 COONH 4 and CH 3 CN:CH 3 OH (90:10, v/v) as the mobile phase under gradient conditions. Detection was performed using tandem mass spectrometry equipped with an electrospray ionization interface in positive ion mode.The selected reaction monitoring transitions for miglitol and a stable isotope‐labeled internal standard were m/z 208 → m/z 146 and m/z 212 → m/z 176, respectively. The correlation coefficients of the calibration curves ranged from 0.9984 to 0.9993 over a concentration range of 0.5–100 ng/mL plasma. The quantification limit of the proposed method was more than 10 times lower than those of previously reported LC‐MS/MS methods. The novel method was successfully validated and applied to a pharmacokinetic study in rats. Copyright © 2014 John Wiley & Sons, Ltd.