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<p>Diabetes mellitus is a widespread chronic disorder commonly associated with poor dietary habits and elevated stress levels. The US Food and Drug Administration (FDA) has recently approved a novel fixed-dose combination therapy containing metformin hydrochloride (MET), sitagliptin phosphate (SITA), and pioglitazone hydrochloride (PIO), providing a new strategy for managing Type 2 diabetes mellitus. This has created a need to establish a precise, sensitive, and validated method for their simultaneous quantification. A literature review revealed that no stability-indicating high-performance thin-layer chromatography (HPTLC) method has been reported for this combination, highlighting the significance of this work. For the separation process, thin-layer chromatography plates coated with silica gel 60 F<sub>254</sub> were used as the stationary phase. A mixture of methanol‒toluene‒ammonia‒acetic acid (7:2.5:0.4:0.2, <i>V/V</i>) was used as the mobile phase. Detection was carried out densitometrically at a wavelength of 254&#xa0;nm. The peaks corresponding to MET, SITA, and PIO were well separated at retention factors (<i>R</i><sub>F</sub>) of 0.45, 0.63, and 0.82, respectively. The developed method demonstrated linearity across the concentration ranges of 1500‒4500&#xa0;ng/band, 300‒900&#xa0;ng/band, and 45‒135&#xa0;ng/band with correlation coefficient (<i>r</i><sup>2</sup>) of 0.9992, 0.9993, and 0.9993 for MET, SITA, and PIO, respectively. The limits of detection (LOD) were determined to be 420.50, 84.50, and 4.73&#xa0;ng/band and the limits of quantification (LOQ) were determined to be 893.50, 179.60, and 10.04&#xa0;ng/band for MET, SITA, and PIO, respectively. The stability study was conducted under acidic, basic, oxidative, neutral, photolytic, and thermal conditions. MET and PIO were found stable in thermal and photolytic conditions, while SITA was stable in neutral condition. The proposed method complies with all International Council for Harmonisation (ICH) guidelines, demonstrating that it is accurate, simple, appropriate, and reliable for determining MET, SITA, and PIO in their combined dosage form.</p>

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Development and validation of a stability-indicating high-performance thin-layer chromatography method for the simultaneous estimation of metformin hydrochloride, sitagliptin phosphate, and pioglitazone hydrochloride in bulk and its tablet dosage form

  • 期刊论文

  • 发表日期：

    2026年3月10日

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  • Arun Maruti Kashid,
  • Aarti Satyanarayan Varma,
  • Aniket Dadaso Pawar,
  • Vaishnavi Gopal Tupkar,
  • Aditya Mahesh Shinde

摘要

Diabetes mellitus is a widespread chronic disorder commonly associated with poor dietary habits and elevated stress levels. The US Food and Drug Administration (FDA) has recently approved a novel fixed-dose combination therapy containing metformin hydrochloride (MET), sitagliptin phosphate (SITA), and pioglitazone hydrochloride (PIO), providing a new strategy for managing Type 2 diabetes mellitus. This has created a need to establish a precise, sensitive, and validated method for their simultaneous quantification. A literature review revealed that no stability-indicating high-performance thin-layer chromatography (HPTLC) method has been reported for this combination, highlighting the significance of this work. For the separation process, thin-layer chromatography plates coated with silica gel 60 F254 were used as the stationary phase. A mixture of methanol‒toluene‒ammonia‒acetic acid (7:2.5:0.4:0.2, V/V) was used as the mobile phase. Detection was carried out densitometrically at a wavelength of 254 nm. The peaks corresponding to MET, SITA, and PIO were well separated at retention factors (RF) of 0.45, 0.63, and 0.82, respectively. The developed method demonstrated linearity across the concentration ranges of 1500‒4500 ng/band, 300‒900 ng/band, and 45‒135 ng/band with correlation coefficient (r2) of 0.9992, 0.9993, and 0.9993 for MET, SITA, and PIO, respectively. The limits of detection (LOD) were determined to be 420.50, 84.50, and 4.73 ng/band and the limits of quantification (LOQ) were determined to be 893.50, 179.60, and 10.04 ng/band for MET, SITA, and PIO, respectively. The stability study was conducted under acidic, basic, oxidative, neutral, photolytic, and thermal conditions. MET and PIO were found stable in thermal and photolytic conditions, while SITA was stable in neutral condition. The proposed method complies with all International Council for Harmonisation (ICH) guidelines, demonstrating that it is accurate, simple, appropriate, and reliable for determining MET, SITA, and PIO in their combined dosage form.