Development and validation of a liquid chromatography–tandem mass spectrometric method for the quantification of 5-thio-d-glucose in rat and human plasma

Mizuno-Yasuhira, Akiko; Jingu, Shigeji; Okuyama, Shigeru

doi:10.1016/j.jchromb.2011.11.037

Cited by 1 publication

(1 citation statement)

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“…In the unique SPE, miglitol would pass through the cartridge, but the cationic interferences causing ion suppression would be retained by the cation‐exchange sorbent that was bonded to the silica surface under conditions where an alkaline solvent was used for PPT and SPE. Furthermore, a nonpolar lipid, which was thought to pass through the cartridge if the sorbent was not mixed‐mode but ion‐exchange only and to cause the deterioration of the analytical column based on the results of our previous research for another monomeric sugar (Mizuno‐Yasuhira et al ., ), should be retained by the octadecyl group that is bonded to the silica surface of the mixed‐mode cartridge. Consequently, the MonoSpin C 18 ‐CX mixed‐mode cartridge, which has an octadecyl group and a sulfonic acid group for cation‐exchange on the surface of its silica monolithic support, along with acetonitrile–28% ammonia solution (98:2, v/v) as a solvent for PPT and preconditioning SPE, were selected.…”

Section: Resultsmentioning

confidence: 99%

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

Mizuno-Yasuhira

Kinoshita

Jingu

et al. 2014

Biomedical Chromatography

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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.

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Section: Resultsmentioning

confidence: 99%