Simultaneous determination of linagliptin and metformin by reverse phase-high performance liquid chromatography method: An application in quantitative analysis of pharmaceutical dosage forms

Abstract

To enhance patient compliance toward treatment in diseases like diabetes, usually a combination of drugs is prescribed. Therefore, an anti-diabetic fixed-dose combination of 2.5 mg of linagliptin 500 mg of metformin was taken for simultaneous estimation of both the drugs by reverse phase-high performance liquid chromatography (RP-HPLC) method. The present study aimed to develop a simple and sensitive RP-HPLC method for the simultaneous determination of linagliptin and metformin in pharmaceutical dosage forms. The chromatographic separation was designed and evaluated by using linagliptin and metformin working standard and sample solutions in the linearity range. Chromatographic separation was performed on a C18 column using a mobile phase of 70:30 (v/v) mixture of methanol and 0.05 M potassium dihydrogen orthophosphate (pH adjusted to 4.6 with orthophosphoric acid) delivered at a flow rate of 0.6 mL/min and UV detection at 267 nm. Linagliptin and metformin shown linearity in the range of 2-12 μg/mL and 400–2400 μg/mL respectively with correlation co-efficient of 0.9996 and 0.9989. The resultant findings analyzed for standard deviation (SD) and relative standard deviation to validate the developed method. The retention time of linagliptin and metformin was found to be 6.3 and 4.6 min and separation was complete in <10 min. The method was validated for linearity, accuracy and precision were found to be acceptable over the linearity range of the linagliptin and metformin. The method was found suitable for the routine quantitative analysis of linagliptin and metformin in pharmaceutical dosage forms.

Application of experimental design in HPLC method optimization and robustness for the simultaneous determination of canagliflozin, empagliflozin, linagliptin, and metformin in tablet

“…In addition, several methods were reported for the simultaneous quantitation of LIG and MEF in pure form, in pharmaceutical dosage form, or in human plasma. These methods include spectrophotometry (Rajendran, 2019), HPLC (Jadhav et al, 2016;Jadhav et al, 2017;K et al, 2019;Prasanna et al, 2015;Sivagami et al, 2020;Swamy & Baba, 2013;Vemula et al, 2015), HPTLC (Rajasekaran et al, 2014;Srivani et al, 2016), or LC-MS/MS (Abbas Moussa et al, 2019).…”

Identification and Structural Characterization of Degradation Products of Linagliptin by Mass Spectrometry Techniques

“…The empirical formula is C 25 H 28 N 8 O 2 and the molecular weight is 472.54 g/mol [ 14 ]. In the available literature, we can only find information about some structures of the resulting degradants [ 15 , 16 , 17 ]. There is a lack of information on a comprehensive analysis of degradation products, as well as proposed structures for the identified impurities.…”

“…There is a lack of information on a comprehensive analysis of degradation products, as well as proposed structures for the identified impurities. Several studies have been conducted on the assessment of linagliptin through liquid chromatography methods, encompassing both HPLC and UPLC, in conjunction with UV or PDA detectors [ 17 , 18 , 19 , 20 , 21 , 22 , 23 , 24 ]. However, there are not many papers related to the identification of impurities.…”

Determination of linagliptin and empagliflozin by UPLC and HPTLC techniques aided by lean six sigma approach

“…According to the literature review it was found that, many analytical techniques have been reported for the determination of EMP and LIN, including UV spectrophotometry (Amrutiya et al, 2017;Ayoub, 2016;Cholke et al, 2019;Padmaja & Veerabhadram, 2015), voltammetry (Naccar, Saleh, Omar, Haredy, & Derayea, 2020), HPTLC (Bhole, Wankhede, & Pandey, 2017;Thakor, Amrutkar, & Chaudhari, 2019), HPLC (Abdel-Ghany, Ayad, & Tadros, 2018Al-Sabti & Harbali, 2020;Attimarad, Nagaraja, Aldhubaib, Nair, & Venugopala, 2014;Basak, Gouru, Bera, & Nagappan, 2019;Donepudi & Achanta, 2018;El-Bagary, Elkady, & Ayoub, 2013;Ganorkar, Askarkar, Gupta, & Milind, 2020;Geetha Swarupa, Lakshmana Rao, Prasad, & Suresh Babu, 2016;Gholami, Bahrami, & Faraji, 2020;Manoel et al, 2020;Naazneen & Sridevi, 2016;Padmaja & Veerabhadram, 2017;Rajbangshi, Alam, Hossain, Islam, & Rouf, 2018;Salapaka et al, 2019;Sharif et al, 2020;Supriya Reddy, Chandan, Sai Charan, & Akshay, 2020;Vemula, Dodda, Balekari, Panga, & Veeresham, 2015;Wattamwar, Mungantiwar, Halde, & Pandita, 2020;Yadav, Dornala, Swain, Prabha, & Samanthula, 2020), UPLC (Ayoub, 2015;Dubey, Singh, Tyagi, Bhardwaj, & Raghav, 2014;Jagadabi, Kumar, Pamidi, Ramaprasad, & Nagaraju, 2018;Madana Gopal & Sridhar, 2017;Nannapaneni, Jalalpure, Muppavarapu, & Sirigiri, 2016)…”