{"title":"稳定性指示高效液相色谱法测定二磷酸伯氨喹在乳质体制剂中的应用","authors":"M. Thakkar, S. Brijesh","doi":"10.4103/2349-3666.240300","DOIUrl":null,"url":null,"abstract":"A novel, rapid, and precise stability-indicating gradient reverse-phase high performance liquid chromatographic method for the quantitative determination of primaquine diphosphate and its impurities was developed and validated. Efficient chromatographic separation was achieved on an Inertsil ODS-3V column (150 mm × 4.6 mm, 5.0 μm) with mobile phase containing phosphate buffer (0.05 M KH2PO4, pH 4.5) in gradient combination with acetonitrile at a flow rate of 1 mL/min and the analyte was monitored using a photo-diode array detector at a wavelength of 254 nm. The forced-degradation of primaquine diphosphate was carried out by exposing it to acidic, basic, neutral, thermal, photolytic, and oxidative stress conditions. The peaks of the degradation products obtained were well resolved from that of primaquine diphosphate, indicating that the method developed was specific and stability-indicating. Further, the method was validated according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines, with respect to parameters such as specificity, precision, linearity, accuracy and robustness. The developed method could also be used for the quantification of primaquine diphosphate encapsulated in niosome formulation.","PeriodicalId":34293,"journal":{"name":"Biomedical Research Journal","volume":null,"pages":null},"PeriodicalIF":0.0000,"publicationDate":"2018-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Stability-indicating HPLC method for primaquine diphosphate: An application to niosomal formulation\",\"authors\":\"M. Thakkar, S. Brijesh\",\"doi\":\"10.4103/2349-3666.240300\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"A novel, rapid, and precise stability-indicating gradient reverse-phase high performance liquid chromatographic method for the quantitative determination of primaquine diphosphate and its impurities was developed and validated. Efficient chromatographic separation was achieved on an Inertsil ODS-3V column (150 mm × 4.6 mm, 5.0 μm) with mobile phase containing phosphate buffer (0.05 M KH2PO4, pH 4.5) in gradient combination with acetonitrile at a flow rate of 1 mL/min and the analyte was monitored using a photo-diode array detector at a wavelength of 254 nm. The forced-degradation of primaquine diphosphate was carried out by exposing it to acidic, basic, neutral, thermal, photolytic, and oxidative stress conditions. The peaks of the degradation products obtained were well resolved from that of primaquine diphosphate, indicating that the method developed was specific and stability-indicating. Further, the method was validated according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines, with respect to parameters such as specificity, precision, linearity, accuracy and robustness. The developed method could also be used for the quantification of primaquine diphosphate encapsulated in niosome formulation.\",\"PeriodicalId\":34293,\"journal\":{\"name\":\"Biomedical Research Journal\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2018-04-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Biomedical Research Journal\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.4103/2349-3666.240300\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Biomedical Research Journal","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.4103/2349-3666.240300","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
摘要
建立了一种快速、精确、稳定指示的梯度反相高效液相色谱法定量测定二磷酸伯氨喹及其杂质。色谱柱为Inertsil ODS-3V (150 mm × 4.6 mm, 5.0 μm),流动相为磷酸缓冲液(0.05 M KH2PO4, pH 4.5),与乙腈梯度结合,流速为1 mL/min,波长为254 nm,采用光电二极管阵列检测器监测。通过将二磷酸伯氨喹暴露于酸性、碱性、中性、热、光解和氧化应激条件下进行强制降解。所得降解产物的峰与二磷酸伯氨喹的峰有很好的分辨,表明所建立的方法具有专属性和稳定性。此外,根据国际人用药品注册技术要求协调会议指南,对该方法进行了特异性、精密度、线性、准确性和鲁棒性等参数的验证。该方法也可用于二磷酸伯氨喹胶囊制剂的定量分析。
Stability-indicating HPLC method for primaquine diphosphate: An application to niosomal formulation
A novel, rapid, and precise stability-indicating gradient reverse-phase high performance liquid chromatographic method for the quantitative determination of primaquine diphosphate and its impurities was developed and validated. Efficient chromatographic separation was achieved on an Inertsil ODS-3V column (150 mm × 4.6 mm, 5.0 μm) with mobile phase containing phosphate buffer (0.05 M KH2PO4, pH 4.5) in gradient combination with acetonitrile at a flow rate of 1 mL/min and the analyte was monitored using a photo-diode array detector at a wavelength of 254 nm. The forced-degradation of primaquine diphosphate was carried out by exposing it to acidic, basic, neutral, thermal, photolytic, and oxidative stress conditions. The peaks of the degradation products obtained were well resolved from that of primaquine diphosphate, indicating that the method developed was specific and stability-indicating. Further, the method was validated according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines, with respect to parameters such as specificity, precision, linearity, accuracy and robustness. The developed method could also be used for the quantification of primaquine diphosphate encapsulated in niosome formulation.