A validated LC-MS/MS method for simultaneous determination of linagliptin and metformin in spiked human plasma coupled with solid phase extraction: Application to a pharmacokinetic study in healthy volunteers

Moussa, Bahia Abbas; Mahrouse, Marianne Alphonse; Fawzy, Michael Gamal

doi:10.1016/j.jpba.2018.09.052

Cited by 42 publications

(24 citation statements)

References 14 publications

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“…In this analysis, the retention time was the shortest, which was comparable to the reported data for MET. It is reported to be at 0.89 min, 15 , 26 at 1.26 min, 41 at 1.4 min, 27 at 1.45 min, 42 1.8 min, 14 at 2.65 min 25 and at 3.1 min. 28 …”

Section: Resultsmentioning

confidence: 95%

“…Until now, only a few LC-MS/MS methods for determining MET have been published in biological samples, such as plasma and serum. 6,[12][13][14][15] Dried blood spot (DBS) screening tests were used in the 1960s to diagnose metabolic disorders (phenylketonuria) in infants. Dried Blood Spot (DBS) has recently become a popular choice for bio sampling and for the therapeutic drug monitoring.…”

Section: Introductionmentioning

confidence: 99%

“…Recently, few sensitive methods were reported for individual estimation of MET using LC-MS/MS. 6,[12][13][14][15][25][26][27][28] Only a few studies published the analysis of MET from DBS utilizing LC-MS/MS. 1,4,[29][30][31][32] This sampling technique (DBS) is also acceptable for infants, which reduces the risk of HIV infection and other infectious pathogens to a minimum.…”

Section: Introductionmentioning

confidence: 99%

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Development and Validation of a Simple and Sensitive LC-MS/MS Method for Quantification of Metformin in Dried Blood Spot Its Application as an Indicator for Medication Adherence

AlQuadeib

Aloudah

Almurshedi

et al. 2021

IJGM

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Metformin (MET), an oral biguanide agent, can improve insulin resistance and decrease hepatic glucose production, leading to a reduction in blood-sugar levels. The objective of the present study was to develop and validate simple and rapid LC-MS/MS method for analysis of MET in dried blood spot (DBS) sample for patient monitoring studies purposes (drug adherence). Methods: The chromatographic separation was achieved with Waters HSS-T3 column using gradient elution of mobile phases of two solvents: 1) solvent A, consisted of 10mM ammonium formate, 0.2% formic acid 1%; and 2) acetonitrile solvent B, contained 0.2% formic acid in acetonitrile at a flow rate of 0.2 mL/min. The total run time was 3.0 min. The effectiveness of chromatographic conditions was optimized, and afatinib was used as the internal standard. The assay method was validated using USP 26 and the ICH guidelines. Results: The method showed good linearity in the range 8-48 ng/mL for MET with correlation coefficient (r) >0.9907. The intra-and inter-day precision values for MET met the acceptance criteria as per regulatory guidelines. MET was stable during the stability studies at ambient temperature 25 °C, at refrigerator 4 °C, at 10 °C autosampler, freeze/thaw cycles and 30 days storage in a freezer at −30 ± 0.5 °C. Conclusion:This method has successfully fulfilled all validation requirements referring to EMA and FDA guidelines, and successfully can be applied for MET adherence study. All the six studied patients were approved to metformin adherence.

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Section: Resultsmentioning

confidence: 95%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Development and Validation of a Simple and Sensitive LC-MS/MS Method for Quantification of Metformin in Dried Blood Spot Its Application as an Indicator for Medication Adherence

AlQuadeib

Aloudah

Almurshedi

et al. 2021

IJGM

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“…In two previous studies concerning metformin, the protonated precursor ion [M + H] + at m/z 130.1 was observed, while the most stable ion product was detected at m/z 60.1, due to the loss of guanidine moiety. Thus, the above transition was used for the quantification of the drug in biological materials [33,34]. The biodegradation of metformin was examined in the study of Markiewicz et al [31].…”

Section: Identification Of Degradation Productsmentioning

confidence: 99%

“…Figure 4 shows the proposed degradation pathways, while Figure 5 shows the proposed degradation pathways. biological materials [33,34]. The biodegradation of metformin was examined in the study of Markiewicz et al [31].…”

Section: Identification Of Degradation Productsmentioning

confidence: 99%

Determination of Chemical Stability of Two Oral Antidiabetics, Metformin and Repaglinide in the Solid State and Solutions Using LC-UV, LC-MS, and FT-IR Methods

et al. 2019

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Firstly, metformin and repaglinide were degraded under high temperature/humidity, UV/VIS light, in different pH and oxidative conditions. Secondly, a new validated LC-UV method was examined, as to whether it validly determined these drugs in the presence of their degradation products and whether it is suitable for estimating degradation kinetics. Finally, the respective LC-MS method was used to identify the degradation products. In addition, using FT-IR method, the stability of metformin and repaglinide was scrutinized in the presence of polyvinylpyrrolidone (PVP), mannitol, magnesium stearate, and lactose. Significant degradation of metformin, following the first order kinetics, was observed in alkaline medium. In the case of repaglinide, the most significant and quickest degradation, following the first order kinetics, was observed in acidic and oxidative media (0.1 M HCl and 3% H2O2). Two new degradation products of metformin and nine new degradation products of repaglinide were detected and identified when the stressed samples were examined by our LC-MS method. What is more, the presence of PVP, mannitol, and magnesium stearate proved to affect the stability of metformin, while repaglinide stability was affected in the presence of PVP and magnesium stearate.

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Novel spectrofluorimetric quantification of linagliptin in biological fluids exploiting its interaction with 4‐chloro‐7‐nitrobenzofurazan

et al. 2020

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Direct determination of linagliptin (LIN) using fluorimetry has been limited because LIN releases a very weak fluorescence signal. Accordingly, it should be derivatized first with a fluorogenic reagent to enhance its fluorescence and consequentially the sensitivity required for its bioanalysis. This is the first description of a spectrofluorimetric method for LIN quantification in human plasma. The suggested method exploits the nucleophilic nature of its amino group to react with 4‐chloro‐7‐nitrobenzofurazan (NBD‐Cl) in borate buffer at pH 8.5 to yield a strong fluorescent product with excitation and emission wavelengths of 459 and 529 nm, respectively. Experimental variables concerning the conditions of reaction and fluorescence intensity were carefully investigated and optimized. The linearity range was from 1.0–100 ng ml−1 with a lower detection limit and a lower quantification limit of 0.60 ng ml−1 and 1.82 ng ml−1, respectively. Validation of the suggested method has been accomplished and the application to LIN analysis in commercial tablets as well as in human plasma resulted in a mean per cent recovery of 100.12 ± 1.57 and 99.65 ± 1.22, respectively. The developed method was proven to be a promising, simple and fast alternative bioanalytical method for LIN quantification in clinical and bioequivalence research.

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A validated LC-MS/MS method for simultaneous determination of linagliptin and metformin in spiked human plasma coupled with solid phase extraction: Application to a pharmacokinetic study in healthy volunteers

Cited by 42 publications

References 14 publications

Development and Validation of a Simple and Sensitive LC-MS/MS Method for Quantification of Metformin in Dried Blood Spot Its Application as an Indicator for Medication Adherence

Development and Validation of a Simple and Sensitive LC-MS/MS Method for Quantification of Metformin in Dried Blood Spot Its Application as an Indicator for Medication Adherence

Determination of Chemical Stability of Two Oral Antidiabetics, Metformin and Repaglinide in the Solid State and Solutions Using LC-UV, LC-MS, and FT-IR Methods

Novel spectrofluorimetric quantification of linagliptin in biological fluids exploiting its interaction with 4‐chloro‐7‐nitrobenzofurazan

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