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.
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 CH3 COONH4 and CH3 CN:CH3 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.
Pharmacokinetics and Metabolism, Drug Safety and Pharmacokinetics Laboratories, Taisho Pharmaceutical Co. Ltd, 1-403, Yoshino-cho, Kita-ku, Saitama-shi, Saitama, 331-9530, Japan.
Akiko
A
Mizuno-Yasuhira
Kohnosuke
K
Kinoshita
Shigeji
S
Jingu
Jun-ichi
J
Yamaguchi
D017485:1-Deoxynojirimycin / Q000031:analogs & derivatives* / Q000097:blood; D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D004355:Drug Stability; D016014:Linear Models; D008297:Male; D051381:Rats; D017207:Rats, Sprague-Dawley; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature
C045621:miglitol; D017485:1-Deoxynojirimycin
LC-MS/MS; SPE; miglitol; monomeric sugar; plasma; quantification