Enhanced LC-MS/MS determination of alogliptin and metformin in plasma: Application to a pharmacokinetic study

Mowaka, Shereen; Elkady, Ehab F.; Elmazar, Mohamed M.; Ayoub, Bassam M.

doi:10.1016/j.microc.2016.10.002

Cited by 35 publications

(22 citation statements)

References 15 publications

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“…Improved performance was obtained in this study using HRMS combined with a HILIC analytical column. In some previous studies, the LLOQ concentration was greater than 5 ng/mL [ 6 , 9 , 10 , 11 , 16 ]. In the Fachi et al paper, when ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QToF-MS) was used to develop an analysis method for quantifying various drugs including metformin in human plasma, the concentration of LLOQ was 250 ng/mL [ 16 ].…”

Section: Discussionmentioning

confidence: 99%

“…The sensitivity and peak shape improved when using acetonitrile with 0.1% formic acid than acetonitrile. Compared with previous studies using liquid–liquid extraction or solid-phase extraction [ 9 ], protein precipitation is a rapid and simple preparation method. Last, the total chromatographic run time in this study was 2 min.…”

Section: Discussionmentioning

confidence: 99%

“…Various bioanalytical methods for the determination of metformin in human-derived materials have been developed, including gas chromatography (GC) with mass spectrometry [ 5 ] and liquid chromatography (LC) with UV detection [ 6 , 7 ] or mass spectrometry [ 8 , 9 , 10 ]. GC methods require a complex derivatization procedure before mass spectrometry to compensate chromatographic issues as low volatility [ 5 ].…”

Section: Introductionmentioning

confidence: 99%

“…The reported LC methods with UV detection have shown higher lower limit of quantification (LLOQ) concentration levels [ 6 , 7 ]. Additionally, LC-tandem mass spectrometry suffers from several disadvantages, such as requiring long chromatographic times [ 8 , 9 , 10 ], a lack of sensitivity [ 9 , 10 , 11 ], and the use of complicated sample preparation procedures, including liquid-liquid extraction [ 9 ].…”

Section: Introductionmentioning

confidence: 99%

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Bioanalytical Method Using Ultra-High-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry (UHPL-CHRMS) for the Detection of Metformin in Human Plasma

et al. 2020

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Metformin is the first-line medicine for the treatment of type 2 diabetes. Drug interactions between metformin and other drugs, food, or beverages cannot only cause changes in the pharmacokinetic profiles but also affect the efficacy of metformin. The purpose of this study was to develop a rapid and reliable bioanalytical method for the detection of plasma metformin concentration in humans. To remove interfering substances in plasma, acidified acetonitrile (acetonitrile containing 0.1% formic acid) was added to samples. Ultra-high-performance liquid chromatography (UHPLC) coupled with high resolution mass spectrometry (HRMS) was used to analyze metformin and its internal standard (metformin-d6). Analyte separation was performed on a BEH HILIC analytical column (100 × 2.1 mm, 1.7 μm) using a gradient elution of 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B). The total chromatographic run time was 2 min. The developed method was validated for its linearity, accuracy and precision, selectivity (signal of interfering substance; analyte, lower limit of quantification (LLOQ) ≤ 20%; IS, IS ≤ 5%), sensitivity (LLOQ, 5 ng/mL; S/N ratio ≥ 10), stability (low quality control (LQC, 15 ng/mL), 2.95–14.19%; high quality control (HQC, 1600 ng/mL), −9.49–15.10%), dilution integrity (diluted QC (4000 ng/mL); 10-folds diluted QC (400 ng/mL); 5-folds diluted QC (800 ng/mL); accuracy, 81.30–91.98%; precision, ≤4.47%), carry-over (signal of double blank; analyte, LLOQ ≤20%; IS, IS ≤5%), and matrix effect (LQC, 10.109%; HQC, 12.271%) under various conditions. The constructed calibration curves were shown linear in the concentration range of 5–2000 ng/mL, with within- and between-run precision values of <8.19% and accuracy in the range of 91.13–105.25%. The plasma metformin concentration of 16 healthy subjects was successfully measured by applying the validated bioanalytical method.

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Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Bioanalytical Method Using Ultra-High-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry (UHPL-CHRMS) for the Detection of Metformin in Human Plasma

et al. 2020

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“…The reported C max of alogliptin is 0.11 µg/mL at a dose of 25 mg [23]. Due to the low C max , determination of alogliptin in plasma necessitated using highly sensitive techniques such as LC-MS/MS after protein precipitation of samples [23][24][25][26]. However, protein precipitation induces ionization suppression in MS detection [27,28] and precludes detection by other less sensitive detectors such as UV.…”

Section: Introductionmentioning

confidence: 99%

Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

Hammad

Abdallah

Bedair

et al. 2020

Preprint

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Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were achieved using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines Q2 (R1). The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 19 ng/mL and limit of quantitation was 60 ng /mL. The method was accurate and precise with a % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

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Spectrofluorometric determination of alogliptin an antidiabetic drug in pure and tablet form using fluorescamine, a fluorogenic agent: application to content uniformity test

et al. 2020

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Alogliptin is an antidiabetic drug that belongs to a group called dipeptidyl peptidase-4 enzyme inhibitors. As the drug contains a primary amino group in its structure, it readily reacts with fluorescamine in slightly alkaline medium (borate buffer, pH 8.8) to form a highly fluorescent product. Emission of this product was measured at 477 nm (λ ex = 387 nm). The linear range between the fluorescence intensity and the drug concentration was 0.1-0.5 μg ml −1 with a good correlation coefficient (0.9986). Limits of detection and quantitation were 22 and 72 ng ml −1 , respectively. Guidelines of the International Conference for Harmonisation were followed to validate the developed method with acceptable results. Alogliptin content was determined successfully in its commercial dosage form using the fluorescamine method with good recovery (98.60-101.26%). The method has excellent levels of accuracy and precision compared with the reported method as assessed using Student's t-test and Fisher's exact test. The method was applied successfully for the content uniformity test with high recovery and low relative standard deviation.

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Enhanced LC-MS/MS determination of alogliptin and metformin in plasma: Application to a pharmacokinetic study

Cited by 35 publications

References 15 publications

Bioanalytical Method Using Ultra-High-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry (UHPL-CHRMS) for the Detection of Metformin in Human Plasma

Bioanalytical Method Using Ultra-High-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry (UHPL-CHRMS) for the Detection of Metformin in Human Plasma

Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

Spectrofluorometric determination of alogliptin an antidiabetic drug in pure and tablet form using fluorescamine, a fluorogenic agent: application to content uniformity test

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