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. 2018 Sep 2:2018:2569027.
doi: 10.1155/2018/2569027. eCollection 2018.

Rapid, Validated UPLC-MS/MS Method for Determination of Glibenclamide in Rat Plasma

Mohd Aftab Alam  1 , Fahad Ibrahim Al-Jenoobi  1 , Abdullah Mohammed Al-Mohizea  1
Affiliations

Rapid, Validated UPLC-MS/MS Method for Determination of Glibenclamide in Rat Plasma

Mohd Aftab Alam et al. Int J Anal Chem. .

Erratum in

Abstract

Quick and specific bioanalytical methods are required for analyzing drugs in biological samples. A simple, quick, sensitive, and specific UPLC-MS/MS method was developed and validated for glibenclamide determination in plasma samples. The plasma samples were processed by protein precipitation technique. Glimepiride was used as internal standard (IS). Glibenclamide and glimepiride were eluted on C18 column (Acquity UPLC®BEH). Mobile phase consisting of acetonitrile (0.1% formic acid) and water (0.1% formic acid) was pumped in binary gradient mode at flow rate of 150 μL/min. Glibenclamide and IS elution time was about 1.0 min, and total run time was 2.0 min. The mass spectrometer (triple-quadrupole) was operated in positive electrospray ionization mode. Sodium adducts [M + Na]+ of glibenclamide and IS were monitored in MRM mode. A linear calibration curve was obtained in the range of 10-1280 ng/mL, with regression equation Y = 0.0076 X - 0.0165 and linear regression coefficient r2 = 0.999. Lower limit of quantitation was 10 ng/mL. Accuracy of the method at LQC, MQC, and HQC was 109.7% (± 6.7), 93.6% (± 0.4), and 99.3% (± 1.9), respectively. The coefficient of variation for precision at all QC concentrations was less than 6%. Recovery at LLQC, MQC, and HQC was 104.2% (± 4.9), 100.6% (± 0.9), and 102.9% (± 5.8), respectively. The method was successfully implemented for pharmacokinetic investigations (in-house data).

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Figures

Figure 1
Figure 1
The representative chromatograms of daughter fragments of glibenclamide and glimepiride.
Figure 2
Figure 2
Transition of glibenclamide sodium adduct to daughter fragment (m/z 516.11 > 391).
Figure 3
Figure 3
Transition of glibenclamide sodium adduct to daughter fragment (m/z 516.11 > 417).
Figure 4
Figure 4
Transition of glimepiride sodium adduct to daughter fragment (m/z 513.19 > 374).
Figure 5
Figure 5
Transition of glimepiride sodium adduct to daughter fragment (m/z 513.19 > 400).
Figure 6
Figure 6
The representative chromatograms of blank plasma sample.
Figure 7
Figure 7
The calibration curve of glibenclamide in plasma.
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References

    1. Khatri J., Qassim S., Abed O., Abraham B., Al-Lami A., Masood S. A novel extractionless HPLC fluorescence method for the determination of glyburide in the human plasma: Application to a bioequivalence study. Journal of Pharmacy & Pharmaceutical Sciences. 2001;4(2):201–206. - PubMed
    1. Hoizey G., Lamiable D., Trenque T., et al. Identification and quantification of 8 sulfonylureas with clinical toxicology interest by liquid chromatography-ion-trap tandem mass spectrometry and library searching. Clinical Chemistry. 2005;51(9):1666–1672. doi: 10.1373/clinchem.2005.050864. - DOI - PubMed
    1. Venkatesh P., Harisudhan T., Choudhury H., Mullangi R., Srinivas N. R. Simultaneous estimation of six anti-diabetic drugs - Glibenclamide, gliclazide, glipizide, pioglitazone, repaglinide and rosiglitazone: Development of a novel HPLC method for use in the analysis of pharmaceutical formulations and its application to human plasma assay. Biomedical Chromatography. 2006;20(10):1043–1048. doi: 10.1002/bmc.635. - DOI - PubMed
    1. Albu F., Georgiţǎ C., David V., Medvedovici A. Determination of glibenclamide in human plasma by liquid chromatography and atmospheric pressure chemical ionization/MS-MS detection. Journal of Chromatography B. 2007;846(1-2):222–229. doi: 10.1016/j.jchromb.2006.09.005. - DOI - PubMed
    1. Georgita C., Albu F., David V., Medvedovici A. Simultaneous assay of metformin and glibenclamide in human plasma based on extraction-less sample preparation procedure and LC/(APCI)MS. Journal of Chromatography B. 2007;854(1-2):211–218. doi: 10.1016/j.jchromb.2007.04.032. - DOI - PubMed

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