{"title":"开发、验证和应用离子对反相液相色谱-串联质谱法定量检测纽西奈森。","authors":"Xiao Zhang, Chunjie Sha, Wei Zhang, Fengjuan Zhao, Mingli Zhu, Guangyi Leng, Wanhui Liu","doi":"10.4155/bio-2023-0218","DOIUrl":null,"url":null,"abstract":"<p><p><b>Background:</b> The fully phosphorothioate-modified oligonucleotide (OGN) nusinersen has low ionization efficiency in the negative ion mode, resulting in a low mass spectrometry response. There have been no relevant reports on developing a LC-MS method for the determination of nusinersen by optimizing mobile phase composition. <b>Materials & methods:</b> Mobile phase additives comprised of 15 mM triethylamine/25 mM 1,1,1,3,3,3-hexafluoro-2-propanol with a pH of 9.6. Nusinersen was extracted from plasma using Oasis<sup>®</sup> HLB solid-phase extraction (Waters, MA, USA). <b>Results & conclusion:</b> By adjusting the pH of the mobile phase to 9.6 by optimizing the type and concentration of ion-pair reagents, a high mass spectrometry response was obtained. The developed method was applied to nusinersen and met the requirements for the pharmacokinetic study of nusinersen in rabbits.</p>","PeriodicalId":8797,"journal":{"name":"Bioanalysis","volume":" ","pages":"305-317"},"PeriodicalIF":1.9000,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development, validation and application of an ion-pair reversed-phase liquid chromatography-tandem mass spectrometry method for the quantification of nusinersen.\",\"authors\":\"Xiao Zhang, Chunjie Sha, Wei Zhang, Fengjuan Zhao, Mingli Zhu, Guangyi Leng, Wanhui Liu\",\"doi\":\"10.4155/bio-2023-0218\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p><b>Background:</b> The fully phosphorothioate-modified oligonucleotide (OGN) nusinersen has low ionization efficiency in the negative ion mode, resulting in a low mass spectrometry response. There have been no relevant reports on developing a LC-MS method for the determination of nusinersen by optimizing mobile phase composition. <b>Materials & methods:</b> Mobile phase additives comprised of 15 mM triethylamine/25 mM 1,1,1,3,3,3-hexafluoro-2-propanol with a pH of 9.6. Nusinersen was extracted from plasma using Oasis<sup>®</sup> HLB solid-phase extraction (Waters, MA, USA). <b>Results & conclusion:</b> By adjusting the pH of the mobile phase to 9.6 by optimizing the type and concentration of ion-pair reagents, a high mass spectrometry response was obtained. The developed method was applied to nusinersen and met the requirements for the pharmacokinetic study of nusinersen in rabbits.</p>\",\"PeriodicalId\":8797,\"journal\":{\"name\":\"Bioanalysis\",\"volume\":\" \",\"pages\":\"305-317\"},\"PeriodicalIF\":1.9000,\"publicationDate\":\"2024-03-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Bioanalysis\",\"FirstCategoryId\":\"3\",\"ListUrlMain\":\"https://doi.org/10.4155/bio-2023-0218\",\"RegionNum\":4,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"2024/2/9 0:00:00\",\"PubModel\":\"Epub\",\"JCR\":\"Q3\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Bioanalysis","FirstCategoryId":"3","ListUrlMain":"https://doi.org/10.4155/bio-2023-0218","RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"2024/2/9 0:00:00","PubModel":"Epub","JCR":"Q3","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
引用次数: 0
摘要
背景：全硫代磷酸酯修饰的寡核苷酸（OGN）nusinersen 在负离子模式下电离效率较低，导致质谱响应较低。目前还没有相关报道介绍如何通过优化流动相组成来开发一种液相色谱-质谱法测定奴西那生。材料与方法：流动相添加剂为 15 mM 三乙胺/25 mM 1,1,1,3,3,3- 六氟-2-丙醇，pH 值为 9.6。使用 Oasis® HLB 固相萃取（美国马萨诸塞州沃特世公司）从血浆中提取奴西那生。结果与结论通过优化离子对试剂的种类和浓度，将流动相的 pH 值调至 9.6，获得了较高的质谱响应。所建立的方法适用于奴西能森，符合兔奴西能森药代动力学研究的要求。
Development, validation and application of an ion-pair reversed-phase liquid chromatography-tandem mass spectrometry method for the quantification of nusinersen.
Background: The fully phosphorothioate-modified oligonucleotide (OGN) nusinersen has low ionization efficiency in the negative ion mode, resulting in a low mass spectrometry response. There have been no relevant reports on developing a LC-MS method for the determination of nusinersen by optimizing mobile phase composition. Materials & methods: Mobile phase additives comprised of 15 mM triethylamine/25 mM 1,1,1,3,3,3-hexafluoro-2-propanol with a pH of 9.6. Nusinersen was extracted from plasma using Oasis® HLB solid-phase extraction (Waters, MA, USA). Results & conclusion: By adjusting the pH of the mobile phase to 9.6 by optimizing the type and concentration of ion-pair reagents, a high mass spectrometry response was obtained. The developed method was applied to nusinersen and met the requirements for the pharmacokinetic study of nusinersen in rabbits.
IF 3.4 4区 生物学ProteomicsPub Date : 2019-12-02DOI: 10.1002/pmic.201970201
Fei-Long Yu, Huan Miao, Jinjin Xia, Fan Jia, Huadong Wang, Fuqiang Xu, Lin Guo
来源期刊
BioanalysisBIOCHEMICAL RESEARCH METHODS-CHEMISTRY, ANALYTICAL
CiteScore
3.30
自引率
16.70%
发文量
88
审稿时长
2 months
期刊介绍：
Reliable data obtained from selective, sensitive and reproducible analysis of xenobiotics and biotics in biological samples is a fundamental and crucial part of every successful drug development program. The same principles can also apply to many other areas of research such as forensic science, toxicology and sports doping testing.
The bioanalytical field incorporates sophisticated techniques linking sample preparation and advanced separations with MS and NMR detection systems, automation and robotics. Standards set by regulatory bodies regarding method development and validation increasingly define the boundaries between speed and quality.
Bioanalysis is a progressive discipline for which the future holds many exciting opportunities to further reduce sample volumes, analysis cost and environmental impact, as well as to improve sensitivity, specificity, accuracy, efficiency, assay throughput, data quality, data handling and processing.
The journal Bioanalysis focuses on the techniques and methods used for the detection or quantitative study of analytes in human or animal biological samples. Bioanalysis encourages the submission of articles describing forward-looking applications, including biosensors, microfluidics, miniaturized analytical devices, and new hyphenated and multi-dimensional techniques.
Bioanalysis delivers essential information in concise, at-a-glance article formats. Key advances in the field are reported and analyzed by international experts, providing an authoritative but accessible forum for the modern bioanalyst.
京公网安备 11010802042870号
京ICP备2023020795号-1
分享
求助内容：
应助结果提醒方式：
扫码关注我们
