Avani Chokshi, A. Gajjar, Pooja Bhanushali, Pritesh Desai
{"title":"人血浆中抗白血病药物达沙替尼的定量:灵敏液相色谱法的应用","authors":"Avani Chokshi, A. Gajjar, Pooja Bhanushali, Pritesh Desai","doi":"10.25135/jcm.64.2108-2174","DOIUrl":null,"url":null,"abstract":"Dasatinib is a tyrosine kinase inhibitor that is approved and prescribed to patients with chronic myelogenous leukemia and Philadelphia chromosome. Present work reports development of reversed-phase high performance liquid chromatographic method for determination of Dasatinib in human plasma and validation of the developed method according to the guidelines provided by European Medicines Agency (EMA). An RP-HPLC method with UV detection and isocratic elution has been developed and validated for analysis of Dasatinib in human plasma over a range of 5-300 ng/mL. Imatinib was used as an internal standard. Both, the drug and the internal standard were separated on the Inertsil C18 column (150 mm×4.6 mm×0.005 mm) using Ammonium Acetate buffer pH 6.4 and acetonitrile at a ratio of 65:35 as mobile phase. The flow rate was adjusted to 0.7 mL min-1. The detection was performed at 310 nm wavelength. Sample pre-purification was performed through simple protein precipitation using acetonitrile followed by sample collection through centrifugation. The developed method was linear in the range of 5-300 ng/mL with correlation coefficients (r) of 0.995. The lower limit of quantification for Dasatinib in plasma was 5 ng/mL. The accuracy and precision of the method were well within the acceptable limits of 15% over the linear range. In general, the developed method is efficient and inexpensive. It is very simple from the extraction of drug from the plasma matrix to the isocratic elution of analytes. From the data, it can be concluded that the developed method is selective, precise and accurate and applicable for the determination of Dasatinib in human plasma samples.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.8000,"publicationDate":"2021-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"2","resultStr":"{\"title\":\"Quantification of antileukemic drug Dasatinib in human plasma: Application of a sensitive liquid chromatographic method\",\"authors\":\"Avani Chokshi, A. Gajjar, Pooja Bhanushali, Pritesh Desai\",\"doi\":\"10.25135/jcm.64.2108-2174\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"Dasatinib is a tyrosine kinase inhibitor that is approved and prescribed to patients with chronic myelogenous leukemia and Philadelphia chromosome. Present work reports development of reversed-phase high performance liquid chromatographic method for determination of Dasatinib in human plasma and validation of the developed method according to the guidelines provided by European Medicines Agency (EMA). An RP-HPLC method with UV detection and isocratic elution has been developed and validated for analysis of Dasatinib in human plasma over a range of 5-300 ng/mL. Imatinib was used as an internal standard. Both, the drug and the internal standard were separated on the Inertsil C18 column (150 mm×4.6 mm×0.005 mm) using Ammonium Acetate buffer pH 6.4 and acetonitrile at a ratio of 65:35 as mobile phase. The flow rate was adjusted to 0.7 mL min-1. The detection was performed at 310 nm wavelength. Sample pre-purification was performed through simple protein precipitation using acetonitrile followed by sample collection through centrifugation. The developed method was linear in the range of 5-300 ng/mL with correlation coefficients (r) of 0.995. The lower limit of quantification for Dasatinib in plasma was 5 ng/mL. The accuracy and precision of the method were well within the acceptable limits of 15% over the linear range. In general, the developed method is efficient and inexpensive. It is very simple from the extraction of drug from the plasma matrix to the isocratic elution of analytes. From the data, it can be concluded that the developed method is selective, precise and accurate and applicable for the determination of Dasatinib in human plasma samples.\",\"PeriodicalId\":15343,\"journal\":{\"name\":\"Journal of Chemical Metrology\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":1.8000,\"publicationDate\":\"2021-10-09\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"2\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chemical Metrology\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.25135/jcm.64.2108-2174\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chemical Metrology","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.25135/jcm.64.2108-2174","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 2
摘要
达沙替尼是一种酪氨酸激酶抑制剂,被批准用于慢性粒细胞白血病和费城染色体患者。目前的工作报告了用于测定人血浆中达沙替尼的反相高效液相色谱法的开发,并根据欧洲药品管理局(EMA)提供的指南对所开发的方法进行了验证。已经开发并验证了一种具有UV检测和等度洗脱的RP-HPLC方法,用于分析5-300 ng/mL范围内的人血浆中的达沙替尼。伊马替尼被用作内标。药物和内标物均在Inertsil C18柱(150mm×4.6mm×0.005mm)上分离,使用醋酸铵缓冲液pH 6.4和乙腈(比例为65:35)作为流动相。将流速调节至0.7 mL min-1。检测波长为310nm。样品预纯化通过使用乙腈的简单蛋白质沉淀进行,然后通过离心收集样品。所开发的方法在5-300 ng/mL范围内呈线性,相关系数(r)为0.995。达沙替尼在血浆中的定量下限为5 ng/mL。该方法的准确度和精密度在线性范围内均在15%的可接受范围内。总的来说,所开发的方法是有效和廉价的。从血浆基质中提取药物到分析物的等度洗脱非常简单。从数据中可以得出结论,该方法具有选择性、精确性和准确性,适用于人血浆样品中达沙替尼的测定。
Quantification of antileukemic drug Dasatinib in human plasma: Application of a sensitive liquid chromatographic method
Dasatinib is a tyrosine kinase inhibitor that is approved and prescribed to patients with chronic myelogenous leukemia and Philadelphia chromosome. Present work reports development of reversed-phase high performance liquid chromatographic method for determination of Dasatinib in human plasma and validation of the developed method according to the guidelines provided by European Medicines Agency (EMA). An RP-HPLC method with UV detection and isocratic elution has been developed and validated for analysis of Dasatinib in human plasma over a range of 5-300 ng/mL. Imatinib was used as an internal standard. Both, the drug and the internal standard were separated on the Inertsil C18 column (150 mm×4.6 mm×0.005 mm) using Ammonium Acetate buffer pH 6.4 and acetonitrile at a ratio of 65:35 as mobile phase. The flow rate was adjusted to 0.7 mL min-1. The detection was performed at 310 nm wavelength. Sample pre-purification was performed through simple protein precipitation using acetonitrile followed by sample collection through centrifugation. The developed method was linear in the range of 5-300 ng/mL with correlation coefficients (r) of 0.995. The lower limit of quantification for Dasatinib in plasma was 5 ng/mL. The accuracy and precision of the method were well within the acceptable limits of 15% over the linear range. In general, the developed method is efficient and inexpensive. It is very simple from the extraction of drug from the plasma matrix to the isocratic elution of analytes. From the data, it can be concluded that the developed method is selective, precise and accurate and applicable for the determination of Dasatinib in human plasma samples.