Simultaneous determination of glimepiride, fluoxetine and their metabolites in human plasma by ultra performance liquid chromatography tandem mass spectrometry
10.13699/j.cnki.1001-6821.2015.18.023
- VernacularTitle:超高液相色谱-质谱法检测人血浆中格列美脲和氟西汀及其代谢产物
- Author:
Li-Man QIAO
1
;
Hao WANG
;
Dan LOU
;
Cheng-Ke HUANG
Author Information
1. 温州医科大学 附属第二医院 药学部
- Keywords:
UPLC-MS/MS;
glimepiride;
hydroxy glimepiride;
fluoxetine;
norfluoxetine
- From:
The Chinese Journal of Clinical Pharmacology
2015;(18):1873-1876
- CountryChina
- Language:Chinese
-
Abstract:
Objective To develop an ultra -high performance liquid chromatography-mass spectrometry method to determination the plasma concentration of glimepiride(GLP), fluoxetine(FLU) and their metabo-lites-hydroxy glimepiride ( M1 ) and norfluoxetine ( NFLU) in human. Methods Midazolam was used as internal standard ( IS ) , plasma was precipited by acetonitrile .Chromatographic separation was carried out on an Acquity UPLC BEH C 18 column.A mixture of acetonitrile-0.1%for-mic acid was used as the mobile phase with the flow rate at 0.45 mL· min-1 , gradient elution.The column temperature was set at 40 ℃.The mass spectrometric analysis was performed using an Acquity Xevo TQD triple quadrupole mass spectrometer coupled with an electro -spray ionization(ESI) source in the positive ion mode.The multiple re-action monitoring was used to determination the drug concentration in the samples.Results The standard curve of GLP , M1, FLU, NFLU were y=1.49 ×10 -2 x +4.23 ×10 -2 ( r =0.999 7 ) , y =0.97 ×10 -2 x -0.26 ×10 -2 ( r =0.999 5 ) , y =1.72 × 10 -2 x +9.48 × 10 -2 ( r=0.999 3 ) , y =8.66 ×10 -2 x -1.05 ×10 -2 ( r =0.999 4 ) ,respectively.The linearities were within the concentration range of 5 -1000 , 2.5 -500 , 1 -200 , 0.5 -100 ng· mL-1 for GLP, M1, FLU and NFLU in human plasma.The recoveries of four analytes were greater than 90%, the intra and inter-day precision were less than 15%.Conclusion The method is simple , rapid and suitable for the quantitative determination of plasma glimepiride , fluoxetine and their metabolites , pharmacokinetic and drug interaction studies.
