Komal Kangne, Mayuri Pandit, Atul Shirkhedkar, Shweta Gunjal, Vilas J. Pise, Akhil Nagar
{"title":"结合分析性、环保性和验证性稳定性，建立了他瓦波罗的分析方法，并通过LC-MS对其降解物进行了研究","authors":"Komal Kangne, Mayuri Pandit, Atul Shirkhedkar, Shweta Gunjal, Vilas J. Pise, Akhil Nagar","doi":"10.1007/s00769-025-01635-z","DOIUrl":null,"url":null,"abstract":"<div><p>Tavaborole (TVB), a benzoboroxole derivative, was approved for treating onychomycosis. Boron’s unique properties, such as variable oxidation states, and stability, require specialized analytical methods. The current RP-HPLC method was developed using eco-friendly solvents, maintaining pH, and providing a sharp peak at 5.7 min at 272 nm. A new NP-HPTLC technique was established employing a mobile phase composed of toluene and methanol, yielding an <i>R</i><sub><i>f</i></sub> value of 0.58 with a similar correlation coefficient of 0.9989 for both methods. The accuracy of TVB for both methods was evaluated at levels of 80 to 120%, providing the %RSD in the range of 0.42 to 0.86% (for HPLC) and 0.95 to 1.50% (for HPTLC). The reproducibility for the two methods was performed in triplicate (30–50 µg/ml) for HPLC and (4000 to 6000 ng/band) for HPTLC, and %RSD was evaluated. Replicates at 20 μg/ml for HPLC and 5000 ng/band for HPLTC show the %RSD of 1.42 and 0.65, respectively. Robustness parameters were evaluated by altering pH, wavelength, and flow rate for HPLC and mobile phase composition, plate saturation time, and development distance for HPTLC. The robustness was evaluated by altering the analyst to calculate a %RSD of 0.88 and 0.31 for HPLC and 0.12 and 0.22 for HPTLC. From the results, all the validation parameters are found within acceptable ranges. TVB showed stability in acidic and basic conditions, with degradation observed only under peroxide treatment. An attempt will be made to identify the probable and major degradants of TVB using LC–MS spectra, which was crucial considering the boron’s chemical properties. The RP-HPLC method was confirmed as environmentally sustainable using the AGREE program metrics. In contrast, the NP-HPTLC method met validation standards but was not considered eco-friendly due to solvent choice. Both methods are suitable for commercial applications.</p><h3>Graphical abstract</h3>\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":454,"journal":{"name":"Accreditation and Quality Assurance","volume":"30 3","pages":"261 - 275"},"PeriodicalIF":1.0000,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Combined analytical, eco-friendly, and validated stability indicating method development of tavaborole with the study of its degradants via LC–MS\",\"authors\":\"Komal Kangne, Mayuri Pandit, Atul Shirkhedkar, Shweta Gunjal, Vilas J. Pise, Akhil Nagar\",\"doi\":\"10.1007/s00769-025-01635-z\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>Tavaborole (TVB), a benzoboroxole derivative, was approved for treating onychomycosis. Boron’s unique properties, such as variable oxidation states, and stability, require specialized analytical methods. The current RP-HPLC method was developed using eco-friendly solvents, maintaining pH, and providing a sharp peak at 5.7 min at 272 nm. A new NP-HPTLC technique was established employing a mobile phase composed of toluene and methanol, yielding an <i>R</i><sub><i>f</i></sub> value of 0.58 with a similar correlation coefficient of 0.9989 for both methods. The accuracy of TVB for both methods was evaluated at levels of 80 to 120%, providing the %RSD in the range of 0.42 to 0.86% (for HPLC) and 0.95 to 1.50% (for HPTLC). The reproducibility for the two methods was performed in triplicate (30–50 µg/ml) for HPLC and (4000 to 6000 ng/band) for HPTLC, and %RSD was evaluated. Replicates at 20 μg/ml for HPLC and 5000 ng/band for HPLTC show the %RSD of 1.42 and 0.65, respectively. Robustness parameters were evaluated by altering pH, wavelength, and flow rate for HPLC and mobile phase composition, plate saturation time, and development distance for HPTLC. The robustness was evaluated by altering the analyst to calculate a %RSD of 0.88 and 0.31 for HPLC and 0.12 and 0.22 for HPTLC. From the results, all the validation parameters are found within acceptable ranges. TVB showed stability in acidic and basic conditions, with degradation observed only under peroxide treatment. An attempt will be made to identify the probable and major degradants of TVB using LC–MS spectra, which was crucial considering the boron’s chemical properties. The RP-HPLC method was confirmed as environmentally sustainable using the AGREE program metrics. In contrast, the NP-HPTLC method met validation standards but was not considered eco-friendly due to solvent choice. 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Combined analytical, eco-friendly, and validated stability indicating method development of tavaborole with the study of its degradants via LC–MS
Tavaborole (TVB), a benzoboroxole derivative, was approved for treating onychomycosis. Boron’s unique properties, such as variable oxidation states, and stability, require specialized analytical methods. The current RP-HPLC method was developed using eco-friendly solvents, maintaining pH, and providing a sharp peak at 5.7 min at 272 nm. A new NP-HPTLC technique was established employing a mobile phase composed of toluene and methanol, yielding an Rf value of 0.58 with a similar correlation coefficient of 0.9989 for both methods. The accuracy of TVB for both methods was evaluated at levels of 80 to 120%, providing the %RSD in the range of 0.42 to 0.86% (for HPLC) and 0.95 to 1.50% (for HPTLC). The reproducibility for the two methods was performed in triplicate (30–50 µg/ml) for HPLC and (4000 to 6000 ng/band) for HPTLC, and %RSD was evaluated. Replicates at 20 μg/ml for HPLC and 5000 ng/band for HPLTC show the %RSD of 1.42 and 0.65, respectively. Robustness parameters were evaluated by altering pH, wavelength, and flow rate for HPLC and mobile phase composition, plate saturation time, and development distance for HPTLC. The robustness was evaluated by altering the analyst to calculate a %RSD of 0.88 and 0.31 for HPLC and 0.12 and 0.22 for HPTLC. From the results, all the validation parameters are found within acceptable ranges. TVB showed stability in acidic and basic conditions, with degradation observed only under peroxide treatment. An attempt will be made to identify the probable and major degradants of TVB using LC–MS spectra, which was crucial considering the boron’s chemical properties. The RP-HPLC method was confirmed as environmentally sustainable using the AGREE program metrics. In contrast, the NP-HPTLC method met validation standards but was not considered eco-friendly due to solvent choice. Both methods are suitable for commercial applications.
期刊介绍：
Accreditation and Quality Assurance has established itself as the leading information and discussion forum for all aspects relevant to quality, transparency and reliability of measurement results in chemical and biological sciences. The journal serves the information needs of researchers, practitioners and decision makers dealing with quality assurance and quality management, including the development and application of metrological principles and concepts such as traceability or measurement uncertainty in the following fields: environment, nutrition, consumer protection, geology, metallurgy, pharmacy, forensics, clinical chemistry and laboratory medicine, and microbiology.
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