Liquid Chromatography–Mass Spectrometry Method for the Estimation of Tacrolimus From Whole Blood Using Novel Time Programming Coupled With Diverter Valve Plumbing to Overcome the Matrix Effect

IF 1.7 4区医学 Q4 BIOCHEMICAL RESEARCH METHODS

Biomedical Chromatography Pub Date : 2025-10-03 DOI:10.1002/bmc.70227

Sajad Khaliq Dar, Arshad H. Khuroo, Mohd. Akhtar, Pravesh Singh

{"title":"Liquid Chromatography–Mass Spectrometry Method for the Estimation of Tacrolimus From Whole Blood Using Novel Time Programming Coupled With Diverter Valve Plumbing to Overcome the Matrix Effect","authors":"Sajad Khaliq Dar, Arshad H. Khuroo, Mohd. Akhtar, Pravesh Singh","doi":"10.1002/bmc.70227","DOIUrl":null,"url":null,"abstract":"<div>\n \n <p>Tacrolimus is an immunosuppressant commonly used for the prevention of allograft rejection in transplant patients. Liquid chromatography mass spectrometry (LC–MS/MS) method was successfully developed and validated for the estimation of tacrolimus from whole blood. The extraction of the drug was achieved with protein precipitation followed by solid phase extraction. Tacrolimus related compound A was used as an internal standard. Electrospray ionization in negative mode and multiple reaction monitoring were used to monitor the ion transitions. The method was validated for the linear range of 0.200 ng/mL to 50.000 ng/mL with a correlation coefficient > 0.99. The matrix effect due to whole blood matrix was resolved using an optimized time programming coupled with diverter valve (Valco-valve) plumbing. The developed method was used to estimate tacrolimus concentrations from whole blood in a bioequivalence study. The clinical sample analysis was completed without any failure, and the study was found to be bioequivalent.</p>\n </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7000,"publicationDate":"2025-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Biomedical Chromatography","FirstCategoryId":"3","ListUrlMain":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bmc.70227","RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}

引用次数: 0

Abstract

Tacrolimus is an immunosuppressant commonly used for the prevention of allograft rejection in transplant patients. Liquid chromatography mass spectrometry (LC–MS/MS) method was successfully developed and validated for the estimation of tacrolimus from whole blood. The extraction of the drug was achieved with protein precipitation followed by solid phase extraction. Tacrolimus related compound A was used as an internal standard. Electrospray ionization in negative mode and multiple reaction monitoring were used to monitor the ion transitions. The method was validated for the linear range of 0.200 ng/mL to 50.000 ng/mL with a correlation coefficient > 0.99. The matrix effect due to whole blood matrix was resolved using an optimized time programming coupled with diverter valve (Valco-valve) plumbing. The developed method was used to estimate tacrolimus concentrations from whole blood in a bioequivalence study. The clinical sample analysis was completed without any failure, and the study was found to be bioequivalent.

Abstract Image

查看原文本刊更多论文

采用新型时间规划耦合分流阀管道的液相色谱-质谱法测定全血中他克莫司的含量以克服基质效应。

他克莫司是一种免疫抑制剂，通常用于预防移植患者的同种异体移植排斥反应。建立了液相色谱-质谱法（LC-MS/MS）测定全血中他克莫司含量的方法。采用蛋白质沉淀法和固相萃取法提取药物。他克莫司相关化合物A作为内标。采用负模式电喷雾电离和多重反应监测来监测离子跃迁。该方法在0.200 ~ 50.000 ng/mL的线性范围内，相关系数> 0.99。利用优化的时间规划和分流阀（Valco-valve）管道解决了全血基质的基质效应。在一项生物等效性研究中，该方法被用于估计他克莫司全血浓度。临床样本分析顺利完成，研究结果具有生物等效性。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

求助全文

约1分钟内获得全文求助全文

来源期刊

Biomedical Chromatography 生物-分析化学

CiteScore

3.60

自引率

5.60%

发文量

268

审稿时长

2.3 months

期刊介绍： Biomedical Chromatography is devoted to the publication of original papers on the applications of chromatography and allied techniques in the biological and medical sciences. Research papers and review articles cover the methods and techniques relevant to the separation, identification and determination of substances in biochemistry, biotechnology, molecular biology, cell biology, clinical chemistry, pharmacology and related disciplines. These include the analysis of body fluids, cells and tissues, purification of biologically important compounds, pharmaco-kinetics and sequencing methods using HPLC, GC, HPLC-MS, TLC, paper chromatography, affinity chromatography, gel filtration, electrophoresis and related techniques.