{"title":"超高效液相色谱法测定原料药中莫茚酮的相关化合物","authors":"Balaji Nagarajan, G. Manoharan, Ganapathy Narayanan Shanmugam, Nataraj Palaniyappan, Abhinav Yarragunta","doi":"10.5155/eurjchem.13.2.180-185.2252","DOIUrl":null,"url":null,"abstract":"Effective chromatographic separation was achieved on a phenyl-hexyl stationary phase (50×2.1 mm, 1.9 micron particles) with the economical and straightforward mobile phase combination delivered in isocratic mode at a flow rate of 0.6 mL/min at 254 nm using a ultra-performance liquid chromatography (UPLC) system. In the developed method, the resolution between molindone and its related compounds was more significant than 2.0. Regression analysis shows an r2 value (correlation coefficient) greater than 0.999 for molindone and its associated compounds. This method could detect related compounds of molindone at a level below 0.009% with respect to a test concentration of 500 µg/mL for a 2.0 µL injection volume. The method has shown good, consistent recoveries for related compounds (90-110%). The test solution was found to be stable in the diluent for 48 hours. The drug was subjected to stress conditions. The mass balance was found to be close to 99.3%.","PeriodicalId":89364,"journal":{"name":"European journal of chemistry (Print)","volume":" ","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Ultra-performance liquid chromatography determination of related compounds of molindone in drug substances\",\"authors\":\"Balaji Nagarajan, G. Manoharan, Ganapathy Narayanan Shanmugam, Nataraj Palaniyappan, Abhinav Yarragunta\",\"doi\":\"10.5155/eurjchem.13.2.180-185.2252\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"Effective chromatographic separation was achieved on a phenyl-hexyl stationary phase (50×2.1 mm, 1.9 micron particles) with the economical and straightforward mobile phase combination delivered in isocratic mode at a flow rate of 0.6 mL/min at 254 nm using a ultra-performance liquid chromatography (UPLC) system. In the developed method, the resolution between molindone and its related compounds was more significant than 2.0. Regression analysis shows an r2 value (correlation coefficient) greater than 0.999 for molindone and its associated compounds. This method could detect related compounds of molindone at a level below 0.009% with respect to a test concentration of 500 µg/mL for a 2.0 µL injection volume. The method has shown good, consistent recoveries for related compounds (90-110%). The test solution was found to be stable in the diluent for 48 hours. The drug was subjected to stress conditions. The mass balance was found to be close to 99.3%.\",\"PeriodicalId\":89364,\"journal\":{\"name\":\"European journal of chemistry (Print)\",\"volume\":\" \",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2022-06-30\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"European journal of chemistry (Print)\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.5155/eurjchem.13.2.180-185.2252\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"European journal of chemistry (Print)","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.5155/eurjchem.13.2.180-185.2252","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
在苯基-己基固定相(50×2.1 mm, 1.9微米颗粒)上实现了有效的色谱分离,使用超高效液相色谱(UPLC)系统以等压模式以0.6 mL/min的流速在254 nm处进行经济直接的流动相组合。在该方法中,莫茚酮与其相关化合物的分离度大于2.0。回归分析表明,莫茚酮及其相关化合物的相关系数r2大于0.999。在2.0µL的进样量下,当检测浓度为500µg/mL时,该方法可检测出莫茚酮相关化合物的含量低于0.009%。该方法对相关化合物的加样回收率为90 ~ 110%。试验溶液在稀释剂中稳定48小时。这种药物受到压力条件的影响。质量平衡接近99.3%。
Ultra-performance liquid chromatography determination of related compounds of molindone in drug substances
Effective chromatographic separation was achieved on a phenyl-hexyl stationary phase (50×2.1 mm, 1.9 micron particles) with the economical and straightforward mobile phase combination delivered in isocratic mode at a flow rate of 0.6 mL/min at 254 nm using a ultra-performance liquid chromatography (UPLC) system. In the developed method, the resolution between molindone and its related compounds was more significant than 2.0. Regression analysis shows an r2 value (correlation coefficient) greater than 0.999 for molindone and its associated compounds. This method could detect related compounds of molindone at a level below 0.009% with respect to a test concentration of 500 µg/mL for a 2.0 µL injection volume. The method has shown good, consistent recoveries for related compounds (90-110%). The test solution was found to be stable in the diluent for 48 hours. The drug was subjected to stress conditions. The mass balance was found to be close to 99.3%.