{"title":"用于分析散装和药物剂型中盐酸多塞平的稳定性指示 RP-HPLC 方法的开发与验证","authors":"R. R.","doi":"10.22159/ijpps.2024v16i4.50126","DOIUrl":null,"url":null,"abstract":"Objective: A simple, reliable, and rapid RP-HPLC method showing stability has been established to detect Doxepin Hydrochloride (DOX) with its degraded products. The proposed method has been validated for specificity, linearity, system suitability, accuracy, precision, robustness, LOD, and LOQ as per ICH guidelines. All parameters were found to be within the accepted limits, affirming the method's reliability.\nMethods: Analysis was conducted using RP-HPLC on a Phenomenex C18 Luna column (250 mm × 4.6 mm id, 5 µm) with a mobile phase comprising methanol, acetonitrile, and buffer (40:30:30, v/v/v) and a flow rate of 0.5 ml/min. The detection was performed with a UV detector set at 254 nm. Diverse methods have been employed to investigate forced degradation studies, including acid-base hydrolysis, photolysis, thermal degradation, and oxidation. These studies were conducted both in bulk and in capsule formulations of DOX.\nResults: The retention time (tR) of DOX was 2.92 minutes, and all parameters met acceptable limit values. The response exhibited linearity over a concentration range of 10 to 50 µg/ml (R2 = 0.9974). The percentage of DOX recovered from the pharmaceutical cream dosage form ranged from 97.67% to 101%. Sensitivity levels for the developed method were indicated by limit of detection (LOD) and limit of quantification (LOQ) values of 0.40–0.50 µg/ml. The proposed method was validated according to ICH guidelines.\nConclusion: Hence, a simple, reliable, accurate, and precise HPLC method was developed, proving suitable for the analysis of DOX in both bulk and commercial formulations.","PeriodicalId":14188,"journal":{"name":"International Journal of Pharmacy and Pharmaceutical Sciences","volume":"211 ","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"STABILITY-INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ANALYSIS OF DOXEPIN HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM\",\"authors\":\"R. R.\",\"doi\":\"10.22159/ijpps.2024v16i4.50126\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"Objective: A simple, reliable, and rapid RP-HPLC method showing stability has been established to detect Doxepin Hydrochloride (DOX) with its degraded products. The proposed method has been validated for specificity, linearity, system suitability, accuracy, precision, robustness, LOD, and LOQ as per ICH guidelines. All parameters were found to be within the accepted limits, affirming the method's reliability.\\nMethods: Analysis was conducted using RP-HPLC on a Phenomenex C18 Luna column (250 mm × 4.6 mm id, 5 µm) with a mobile phase comprising methanol, acetonitrile, and buffer (40:30:30, v/v/v) and a flow rate of 0.5 ml/min. The detection was performed with a UV detector set at 254 nm. Diverse methods have been employed to investigate forced degradation studies, including acid-base hydrolysis, photolysis, thermal degradation, and oxidation. These studies were conducted both in bulk and in capsule formulations of DOX.\\nResults: The retention time (tR) of DOX was 2.92 minutes, and all parameters met acceptable limit values. The response exhibited linearity over a concentration range of 10 to 50 µg/ml (R2 = 0.9974). The percentage of DOX recovered from the pharmaceutical cream dosage form ranged from 97.67% to 101%. Sensitivity levels for the developed method were indicated by limit of detection (LOD) and limit of quantification (LOQ) values of 0.40–0.50 µg/ml. The proposed method was validated according to ICH guidelines.\\nConclusion: Hence, a simple, reliable, accurate, and precise HPLC method was developed, proving suitable for the analysis of DOX in both bulk and commercial formulations.\",\"PeriodicalId\":14188,\"journal\":{\"name\":\"International Journal of Pharmacy and Pharmaceutical Sciences\",\"volume\":\"211 \",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2024-04-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"International Journal of Pharmacy and Pharmaceutical Sciences\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.22159/ijpps.2024v16i4.50126\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"International Journal of Pharmacy and Pharmaceutical Sciences","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.22159/ijpps.2024v16i4.50126","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
目的:建立了一种简单、可靠、快速且稳定的 RP-HPLC 方法,用于检测盐酸多塞平(DOX)及其降解产物。根据 ICH 指南,对该方法的特异性、线性、系统适用性、准确度、精密度、稳健性、LOD 和 LOQ 进行了验证。所有参数均在可接受的范围内,证明了该方法的可靠性:分析采用 RP-HPLC 法,使用 Phenomenex C18 Luna 色谱柱(250 mm × 4.6 mm id,5 µm),流动相为甲醇、乙腈和缓冲液(40:30:30,v/v/v),流速为 0.5 ml/min。紫外检测器的检测波长为 254 纳米。强制降解研究采用了多种方法,包括酸碱水解、光解、热降解和氧化。这些研究是在 DOX 的散装和胶囊制剂中进行的:DOX 的保留时间(tR)为 2.92 分钟,所有参数均符合可接受的限值。在 10 至 50 µg/ml 的浓度范围内,反应呈线性关系(R2 = 0.9974)。药膏剂型中 DOX 的回收率为 97.67% 至 101%。该方法的灵敏度为检出限(LOD)和定量限(LOQ)均为0.40-0.50 µg/ml。根据 ICH 指南对所提出的方法进行了验证:因此,所开发的高效液相色谱法简单、可靠、准确、精密,适用于散装和商业制剂中 DOX 的分析。
STABILITY-INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ANALYSIS OF DOXEPIN HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM
Objective: A simple, reliable, and rapid RP-HPLC method showing stability has been established to detect Doxepin Hydrochloride (DOX) with its degraded products. The proposed method has been validated for specificity, linearity, system suitability, accuracy, precision, robustness, LOD, and LOQ as per ICH guidelines. All parameters were found to be within the accepted limits, affirming the method's reliability.
Methods: Analysis was conducted using RP-HPLC on a Phenomenex C18 Luna column (250 mm × 4.6 mm id, 5 µm) with a mobile phase comprising methanol, acetonitrile, and buffer (40:30:30, v/v/v) and a flow rate of 0.5 ml/min. The detection was performed with a UV detector set at 254 nm. Diverse methods have been employed to investigate forced degradation studies, including acid-base hydrolysis, photolysis, thermal degradation, and oxidation. These studies were conducted both in bulk and in capsule formulations of DOX.
Results: The retention time (tR) of DOX was 2.92 minutes, and all parameters met acceptable limit values. The response exhibited linearity over a concentration range of 10 to 50 µg/ml (R2 = 0.9974). The percentage of DOX recovered from the pharmaceutical cream dosage form ranged from 97.67% to 101%. Sensitivity levels for the developed method were indicated by limit of detection (LOD) and limit of quantification (LOQ) values of 0.40–0.50 µg/ml. The proposed method was validated according to ICH guidelines.
Conclusion: Hence, a simple, reliable, accurate, and precise HPLC method was developed, proving suitable for the analysis of DOX in both bulk and commercial formulations.