{"title":"同时测定Fosaprepitant二聚氨胺原料药中8种有关物质的高效液相色谱方法的建立与验证","authors":"Zhiling Cao, Ling Zhang, Maolong Huang, Siyi Xia, Yuhan Sun, Xudong Yu, Dahua Shi, Jian Zhu, Fan Xu","doi":"10.1007/s10337-025-04389-5","DOIUrl":null,"url":null,"abstract":"<div><p>The purpose of this study was to develop and validate a robust, precise, and selective high-performance liquid chromatography (HPLC) method for the separation and determination of related impurities in fosaprepitant dimeglumine API. The chromatographic separation was performed on a Supersil ODS-2 column (250 × 4.6 mm, 5 µm) at a wavelength of 215 nm using a mixture of phosphate buffer (pH 2.15) and acetonitrile as the mobile phase in gradient elution mode. The validation results demonstrate that the method exhibits acceptable specificity, linearity, accuracy, precision, and robustness. The detection limits and quantitation limits ranged from 1.5 to 12.5 ng mL<sup>−1</sup> and from 3.0 to 37.5 ng mL<sup>−1</sup>, respectively. A linear relationship was observed between the peak area and concentration of fosaprepitant and its eight related impurities with a correlation coefficient value of <i>r</i><sup>2</sup> ≥ 0.999. The analysis of commercial fosaprepitant dimeglumine products revealed a significantly higher purity than expected, with all known impurities falling below specification limits. The new HPLC method has been successfully applied to analyze commercial bulk drug samples and is suitable for quality-control laboratories for both qualitative and quantitative assessment of eight related substances in the fosaprepitant dimeglumine API.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 3","pages":"205 - 214"},"PeriodicalIF":1.2000,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development and Validation of an HPLC Method for the Simultaneous Determination of Eight Related Substances in Fosaprepitant Dimeglumine API\",\"authors\":\"Zhiling Cao, Ling Zhang, Maolong Huang, Siyi Xia, Yuhan Sun, Xudong Yu, Dahua Shi, Jian Zhu, Fan Xu\",\"doi\":\"10.1007/s10337-025-04389-5\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>The purpose of this study was to develop and validate a robust, precise, and selective high-performance liquid chromatography (HPLC) method for the separation and determination of related impurities in fosaprepitant dimeglumine API. The chromatographic separation was performed on a Supersil ODS-2 column (250 × 4.6 mm, 5 µm) at a wavelength of 215 nm using a mixture of phosphate buffer (pH 2.15) and acetonitrile as the mobile phase in gradient elution mode. The validation results demonstrate that the method exhibits acceptable specificity, linearity, accuracy, precision, and robustness. The detection limits and quantitation limits ranged from 1.5 to 12.5 ng mL<sup>−1</sup> and from 3.0 to 37.5 ng mL<sup>−1</sup>, respectively. A linear relationship was observed between the peak area and concentration of fosaprepitant and its eight related impurities with a correlation coefficient value of <i>r</i><sup>2</sup> ≥ 0.999. The analysis of commercial fosaprepitant dimeglumine products revealed a significantly higher purity than expected, with all known impurities falling below specification limits. The new HPLC method has been successfully applied to analyze commercial bulk drug samples and is suitable for quality-control laboratories for both qualitative and quantitative assessment of eight related substances in the fosaprepitant dimeglumine API.</p></div>\",\"PeriodicalId\":518,\"journal\":{\"name\":\"Chromatographia\",\"volume\":\"88 3\",\"pages\":\"205 - 214\"},\"PeriodicalIF\":1.2000,\"publicationDate\":\"2025-02-06\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Chromatographia\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1007/s10337-025-04389-5\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Chromatographia","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1007/s10337-025-04389-5","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
引用次数: 0
摘要
本研究的目的是建立和验证一种可靠、精确、选择性强的高效液相色谱（HPLC）方法，用于分离和测定fosaprepitant二聚氨胺原料药中相关杂质。色谱柱为Supersil ODS-2 (250 × 4.6 mm, 5µm)，波长为215 nm，流动相为磷酸缓冲液（pH为2.15）和乙腈，梯度洗脱。验证结果表明，该方法具有可接受的特异性、线性度、准确度、精密度和鲁棒性。检测限为1.5 ~ 12.5 ng mL−1，定量限为3.0 ~ 37.5 ng mL−1。fosaprepitant及其8种杂质峰面积与浓度呈线性关系，相关系数r2≥0.999。对商业磷吡坦二聚氨胺产品的分析显示，其纯度明显高于预期，所有已知杂质均低于规格限制。该方法已成功地应用于商品原料药样品的分析，适用于质量控制实验室对fosaprepitant二聚氨胺原料药中8种相关物质的定性和定量评价。
Development and Validation of an HPLC Method for the Simultaneous Determination of Eight Related Substances in Fosaprepitant Dimeglumine API
The purpose of this study was to develop and validate a robust, precise, and selective high-performance liquid chromatography (HPLC) method for the separation and determination of related impurities in fosaprepitant dimeglumine API. The chromatographic separation was performed on a Supersil ODS-2 column (250 × 4.6 mm, 5 µm) at a wavelength of 215 nm using a mixture of phosphate buffer (pH 2.15) and acetonitrile as the mobile phase in gradient elution mode. The validation results demonstrate that the method exhibits acceptable specificity, linearity, accuracy, precision, and robustness. The detection limits and quantitation limits ranged from 1.5 to 12.5 ng mL−1 and from 3.0 to 37.5 ng mL−1, respectively. A linear relationship was observed between the peak area and concentration of fosaprepitant and its eight related impurities with a correlation coefficient value of r2 ≥ 0.999. The analysis of commercial fosaprepitant dimeglumine products revealed a significantly higher purity than expected, with all known impurities falling below specification limits. The new HPLC method has been successfully applied to analyze commercial bulk drug samples and is suitable for quality-control laboratories for both qualitative and quantitative assessment of eight related substances in the fosaprepitant dimeglumine API.
期刊介绍：
Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.
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