Wanyu Wang, Zhichao Yin, Pengfei Du, Jianbang Wu, Minhui Wang, Yaqin Wang, Ping Wu, Xiaocui Xia, Lin Zhang, Yamin Liu, Zhenyue Gao, Jie Shen, Yuanwei Jia
{"title":"SIL-IS UPLC-APCI-MS/MS法测定人血浆中艾尔地骨糖醇的药代动力学研究。","authors":"Wanyu Wang, Zhichao Yin, Pengfei Du, Jianbang Wu, Minhui Wang, Yaqin Wang, Ping Wu, Xiaocui Xia, Lin Zhang, Yamin Liu, Zhenyue Gao, Jie Shen, Yuanwei Jia","doi":"10.1016/j.jchromb.2025.124468","DOIUrl":null,"url":null,"abstract":"<p><p>Eldecalcitol is a novel analog of 1α,25-dihydroxyvitamin D<sub>3</sub> [1,25(OH)<sub>2</sub>D<sub>3</sub>] for the treatment of patients with osteoporosis. A highly sensitive and specific ultra-performance liquid chromatography coupled to atmospheric pressure chemical ionization tandem mass spectrometry (UPLC-APCI-MS/MS) technique featuring a lower limit of quantitation (LLOQ) as low as 5 pg/ml, has been established and validated for the rapid and accurate quantification of eldecalcitol in human plasma samples. Plasma samples were extracted by solid phase extraction (SPE). Stable isotope-labeled compound eldecalcitol-d6 was used as an internal standard (SIL-IS). The detection process was carried out utilizing Multi-Reaction Monitoring (MRM) mode, employing an atmospheric pressure chemical ionization (APCI) source operating in the positive ion modality. The target fragment ion pairs for eldecalcitol and SIL-IS were identified as m/z 508.6 transitioning to 397.4, and m/z 514.6 transitioning to 403.3, respectively. This method was validated regarding selectivity, LLOQ, linearity, accuracy and precision, recovery, matrix effects, dilution reliability, stability, carryover test, and incurred sample reanalysis (ISR). This methodology had been successfully employed to assess the pharmacokinetics (PK) profile of eldecalcitol in a clinical investigation.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1252 ","pages":"124468"},"PeriodicalIF":2.8000,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Determination of eldecalcitol in human plasma by SIL-IS UPLC-APCI-MS/MS method for pharmacokinetics study.\",\"authors\":\"Wanyu Wang, Zhichao Yin, Pengfei Du, Jianbang Wu, Minhui Wang, Yaqin Wang, Ping Wu, Xiaocui Xia, Lin Zhang, Yamin Liu, Zhenyue Gao, Jie Shen, Yuanwei Jia\",\"doi\":\"10.1016/j.jchromb.2025.124468\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>Eldecalcitol is a novel analog of 1α,25-dihydroxyvitamin D<sub>3</sub> [1,25(OH)<sub>2</sub>D<sub>3</sub>] for the treatment of patients with osteoporosis. A highly sensitive and specific ultra-performance liquid chromatography coupled to atmospheric pressure chemical ionization tandem mass spectrometry (UPLC-APCI-MS/MS) technique featuring a lower limit of quantitation (LLOQ) as low as 5 pg/ml, has been established and validated for the rapid and accurate quantification of eldecalcitol in human plasma samples. Plasma samples were extracted by solid phase extraction (SPE). Stable isotope-labeled compound eldecalcitol-d6 was used as an internal standard (SIL-IS). The detection process was carried out utilizing Multi-Reaction Monitoring (MRM) mode, employing an atmospheric pressure chemical ionization (APCI) source operating in the positive ion modality. The target fragment ion pairs for eldecalcitol and SIL-IS were identified as m/z 508.6 transitioning to 397.4, and m/z 514.6 transitioning to 403.3, respectively. This method was validated regarding selectivity, LLOQ, linearity, accuracy and precision, recovery, matrix effects, dilution reliability, stability, carryover test, and incurred sample reanalysis (ISR). This methodology had been successfully employed to assess the pharmacokinetics (PK) profile of eldecalcitol in a clinical investigation.</p>\",\"PeriodicalId\":348,\"journal\":{\"name\":\"Journal of Chromatography B\",\"volume\":\"1252 \",\"pages\":\"124468\"},\"PeriodicalIF\":2.8000,\"publicationDate\":\"2025-01-13\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chromatography B\",\"FirstCategoryId\":\"1\",\"ListUrlMain\":\"https://doi.org/10.1016/j.jchromb.2025.124468\",\"RegionNum\":3,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography B","FirstCategoryId":"1","ListUrlMain":"https://doi.org/10.1016/j.jchromb.2025.124468","RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
Determination of eldecalcitol in human plasma by SIL-IS UPLC-APCI-MS/MS method for pharmacokinetics study.
Eldecalcitol is a novel analog of 1α,25-dihydroxyvitamin D3 [1,25(OH)2D3] for the treatment of patients with osteoporosis. A highly sensitive and specific ultra-performance liquid chromatography coupled to atmospheric pressure chemical ionization tandem mass spectrometry (UPLC-APCI-MS/MS) technique featuring a lower limit of quantitation (LLOQ) as low as 5 pg/ml, has been established and validated for the rapid and accurate quantification of eldecalcitol in human plasma samples. Plasma samples were extracted by solid phase extraction (SPE). Stable isotope-labeled compound eldecalcitol-d6 was used as an internal standard (SIL-IS). The detection process was carried out utilizing Multi-Reaction Monitoring (MRM) mode, employing an atmospheric pressure chemical ionization (APCI) source operating in the positive ion modality. The target fragment ion pairs for eldecalcitol and SIL-IS were identified as m/z 508.6 transitioning to 397.4, and m/z 514.6 transitioning to 403.3, respectively. This method was validated regarding selectivity, LLOQ, linearity, accuracy and precision, recovery, matrix effects, dilution reliability, stability, carryover test, and incurred sample reanalysis (ISR). This methodology had been successfully employed to assess the pharmacokinetics (PK) profile of eldecalcitol in a clinical investigation.
期刊介绍：
The Journal of Chromatography B publishes papers on developments in separation science relevant to biology and biomedical research including both fundamental advances and applications. Analytical techniques which may be considered include the various facets of chromatography, electrophoresis and related methods, affinity and immunoaffinity-based methodologies, hyphenated and other multi-dimensional techniques, and microanalytical approaches. The journal also considers articles reporting developments in sample preparation, detection techniques including mass spectrometry, and data handling and analysis.
Developments related to preparative separations for the isolation and purification of components of biological systems may be published, including chromatographic and electrophoretic methods, affinity separations, field flow fractionation and other preparative approaches.
Applications to the analysis of biological systems and samples will be considered when the analytical science contains a significant element of novelty, e.g. a new approach to the separation of a compound, novel combination of analytical techniques, or significantly improved analytical performance.
求助内容：
应助结果提醒方式：
京公网安备 11010802042870号
