Quantitative determination of metformin, saxagliptin and 5-hydroxy saxagliptin simultaneously by hydrophilic interaction liquid chromatography - electrospray ionization mass spectrometry and its application to a bioequivalence study with a single-pill combination in human

Peng, Ying; Chang, Qingqing; Yang, Na; Gu, Shiyin; Zhou, Yi; Yin, Lifang; Aa, Jiye; Wang, Guangji

doi:10.1016/j.jchromb.2018.02.007

Cited by 13 publications

(7 citation statements)

References 42 publications

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“…Previously established chromatographic methods were evaluated in terms of their capabilities for concurrent estimation of both SXP and MET; included RP-HPLC (Gedawy et al, 2019), HILIC (AbuRuz et al, 2003;Peng et al, 2018), and capillary electrophoresis (CE) (Maher et al, 2019) techniques. Importantly, the selected amines resolving capacity; resolution (R s ) and capacity factor (K') was the optimum in SCX method (60.52%), followed by RP-HPLC (50.79%) and CE while the lowest was observed for HILIC (50.83%); even it had the worst orthogonal selectivities relative to the RP-HPLC.…”

Section: Resultsmentioning

confidence: 99%

“…The forced degradation studies using SCX chromatography revealed the possible disintegration of SXP and MET under the influence of stress factors like acid-base strength, peroxide, and thermal environment (Prasad et al, 2015) (Fig. 6).…”

Section: Forced Degradation Studiesmentioning

confidence: 99%

“…Second, eventhough to encourage the drug-ODS interaction, the "ion suppression effects" with additional basic buffers further exhibit the peak tailing or fronting effects and, therefore, it disrupt the elution order and selectivities (Buszewska-Forajta et al, 2018). These challenges specifically observed in simultaneous investigation of two or more polar aliphatic amines (Porwal & Talele, 2017). Nonetheless, some other analytical techniques were recommended and demonstrated which predominantly included the hydrophilic interaction liquid chromatography (HILIC) (Peng et al, 2018), capillary zone electrophoresis, high performance thin layer chromatography (Maher et al, 2019;Patel et al, 2017), and supercritical fluid chromatography (Bui et al, 2008) but their significance in polar amines separation is still questionable.…”

Section: Introductionmentioning

confidence: 99%

“…This strong cation exchange (SCX) based chromatography is complementary to the RP-HPLC which however did not use the ion exchange mechanism. Moreover, multiple pharmaceutical drugs and natural products analysis usually required highly sophisticated methods, owing to the involvement with their complexities and most often, low abundance of UV-Visible detection sensitivity (Prasad et al, 2015;Yunoos and Sankar, 2015).…”

Section: Introductionmentioning

confidence: 99%

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Strong cation exchange chromatography: a new option for concurrent quantification of saxagliptin and metformin

Manohar¹,

Kailas²

2021

J Appl Pharm Sci

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Extremely polar antidiabetic drug like metformin (MET) along with saxagliptin (SXP) often suffer from peak fronting/ tailing effects along with earlier elution with void volume in RP-HPLC. Therefore, alternative and complimentary to this RP-HPLC, the strong cation exchange (SCX) chromatography has been used for the simultaneous quantification of SXP and MEt along with stability studies. This investigation was performed on the Phenomenex Luna SCX column (100 × 2.1 mm. id, 5 μm) where both SXP and MET were eluted with ammonium formate (15 mM):MeOH (83:17 v/v) for 10 minutes with isocratic elution at 1 ml/minutes flow rate and performed at 30°C, and monitored at 230 and 260 nm wavelength where the retention time of both SXP and MET were 2.290 and 3.520 minutes, respectively. The validation studies revealed good linearity over the concentration ranging between 35.5 and 500 μg/ml for SXP and 15.5-250 μg/ml for MET with r 2 values were 1.00 and 0.999 respectively. The percentage (%) recoveries for SXP and MET were 100.37% (±1.24) and 100.39% (±1.22), respectively. Moreover, as resulted, the acid, peroxide and thermal induced stress conditions have not made any significant changes but 0.1N NaOH at 50°C induced the degradation of SXP and MET.

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Section: Resultsmentioning

confidence: 99%

Section: Forced Degradation Studiesmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Strong cation exchange chromatography: a new option for concurrent quantification of saxagliptin and metformin

Manohar¹,

Kailas²

2021

J Appl Pharm Sci

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“…20,21,24 These methods are available for quantification of EM with other drugs like linagliptin, 20 piglitazone with its M III and M IV metabolites 21 and glimepiride. 25 Similarly, various bioanalytical methods are available for the quantification of ME with other drugs like gliptins, [26][27][28][29][30] statins, 31 biguanides, 32 and gliflozins. 33,34 A detailed comparison of methods developed for the determination of EM and ME is illustrated in Table 1.…”

Section: Introductionmentioning

confidence: 99%

Development of simultaneous determination of empagliflozin and metformin in human plasma using liquid chromatography–mass spectrometry and application to pharmacokinetics

Wattamwar

Mungantiwar²,

Halde³

et al. 2019

Eur J Mass Spectrom (Chichester)

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A rapid and sensitive liquid chromatography–mass spectrometry method was developed, optimized, and validated for simultaneous quantification of empagliflozin and metformin in human plasma using empagliflozin D4and metformin D6 as an internal standard. Analytes and internal standard were extracted from plasma by optimized solid-phase extraction technique using Strata X polymeric reverse phase (30 mg-1cc) solid-phase extraction cartridges. The prepared samples were chromatographed on Orosil C18 column (150 × 4.6 mm, 3 µ). Separation was done by pumping isocratic mobile phase consisting of methanol and 10 mM ammonium trifluoroacetate (90:10, v/v) in positive ion mode at a flow rate of 0.8 mL/min. The API 3200 liquid chromatography–mass spectrometry system having turbo ion spray as an ion source coupled with Shimadzu Prominence ultrafast liquid chromatography system was operated under the selected reaction monitoring mode. Turbo ion spray ionization was used for mass transition of m/z 468.070/355.100 and m/z 130.072/71.200 for empagliflozin and metformin, respectively. A method was successfully validated for concentration range of 10.09–5013.46 ng/mL for both the analytes and according to the United States Food and Drugs Administration guidelines. The linearity was found to be in the range of 10.09–403.46 ng/mL for empagliflozin and 25.44–5013.46 ng/mL for metformin. The limit of quantification was found to be 10.09 ng/mL for empagliflozin and 25.44 ng/mL for metformin. Intra- and inter-day/between batch precision determination for empagliflozin and metformin, expressed as coefficient of variation were within the acceptance limits and ranged below 13.16%. A short run time of 3.3 min allows analysis of more than 400 plasma samples per day. The developed method was successfully applied to fasting pharmacokinetic study in healthy human volunteers. Results of incurred sample re-analysis were within the acceptance range of ±20% of original value, for 97.2% of samples reanalyzed for empagliflozin and 100% of samples reanalyzed for metformin.

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Ion-pair solid phase extraction for the simultaneous separation and quantitation of metformin and canagliflozin in human plasma by LC-MS/MS

Shah

Shrivastav

2018

Microchemical Journal

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Quantitative determination of metformin, saxagliptin and 5-hydroxy saxagliptin simultaneously by hydrophilic interaction liquid chromatography - electrospray ionization mass spectrometry and its application to a bioequivalence study with a single-pill combination in human

Cited by 13 publications

References 42 publications

Strong cation exchange chromatography: a new option for concurrent quantification of saxagliptin and metformin

Strong cation exchange chromatography: a new option for concurrent quantification of saxagliptin and metformin

Development of simultaneous determination of empagliflozin and metformin in human plasma using liquid chromatography–mass spectrometry and application to pharmacokinetics

Ion-pair solid phase extraction for the simultaneous separation and quantitation of metformin and canagliflozin in human plasma by LC-MS/MS

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