Article(id=1291404326874895096, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1291404284806030089, articleNumber=null, orderNo=null, doi=10.13699/j.cnki.1001-6821.2025.04.020, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1722355200000, receivedDateStr=2024-07-31, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1785824384659, onlineDateStr=2026-08-04, pubDate=1740672000000, pubDateStr=2025-02-28, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1785824384659, onlineIssueDateStr=2026-08-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1785824384659, creator=13701087609, updateTime=1785824384659, updator=13701087609, issue=Issue{id=1291404284806030089, tenantId=1146029695717560320, journalId=1246415772164075586, year='2025', volume='41', issue='4', pageStart='451', pageEnd='600', issueExtLink='null', onlineDate='null', pubDate='1740672000000', pubDateStr='2025-02-28', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1785824374629, creator='13701087609', updateTime=1785824374629, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=548, endPage=551, ext={EN=ArticleExt(id=1291404327051055865, articleId=1291404326874895096, tenantId=1146029695717560320, journalId=1246415772164075586, language=EN, title=Hollow fiber centrifugal ultrafiltration for the determination of free methotrexate concentration in human plasma, columnId=1246531413395263850, journalTitle=Chinese Journal of Clinical Pharmacology, columnName=Research Method, runingTitle=null, highlight=null, articleAbstract=
Objective To establish a hollow fiber centrifugal ultrafiltration (HFCF-UF) coupled with ultra-high performance liquid chromatography (UPLC) method for the analysis of free methotrexate (MTX) concentration in human plasma and apply to clinical therapeutic drug monitoring.
Methods Plasma samples 500 μL were prepared with HFCF-UF. A Waters UPLC BEH C18 column (50.0 mm×2.1 mm, 1.7 μm) was used. The mobile phase consisted of methanol and 0.05 mol·L-1 phosphate buffer (pH 6.2) (17∶83, v/v) at a flow rate of 0.2 mL·min-1. The column temperature was maintained at 30 ℃. The detected wavelength was 302 nm. The specificity, linear relationship, lower limit of quantification (LLOQ), precision, recovery rate and stability of this method were investigated, and it was applied to the determination of clinical plasma samples.
Results The good linear relationship were obtained between concentration of free MTX in human plasma from 0.05-10.00 μmol·L-1, y=0.297x+0.001 (r2=0.999). The LLOQ of MTX free plasma concentration analysis was 0.05 μmol·L-1. The method recovery rates of free MTX were 95.77%-100.52%. The absolute recovery rates of free MTX was 84.09%-92.93%. The intra-day and inter-day relative standard deviation (RSD) were all less than 7.0 %. It was successfully used to analyze free MTX concentration in 52 plasma samples from patients with MTX chemotherapy. The average free plasma concentration of MTX in these 52 patients was 0.68 μmol·L-1, with the maximum value of 9.32 μmol·L-1 and the minimum value of 0.056 μmol·L-1.
Conclusion The developed method is simple, accurate and sensitive, which is suitable for the analysis of free MTX on clinical therapeutic drug monitoring.
, authors=Wei-chong DONG
1, Jia-liang GUO
2, Shuai-shuai GAO
1, Hao-ran LI
1, Fang-ting LI
1, Ye JIANG
3, Zhi-qing ZHANG
1, authorsList=Wei-chong DONG, Jia-liang GUO, Shuai-shuai GAO, Hao-ran LI, Fang-ting LI, Ye JIANG, Zhi-qing ZHANG, authorCompany=null, correspAuthors=Zhi-qing ZHANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1291404327814419194, articleId=1291404326874895096, tenantId=1146029695717560320, journalId=1246415772164075586, language=CN, title=用中空纤维离心超滤法测定人血浆中甲氨蝶呤的游离浓度, columnId=1246531413600784769, journalTitle=中国临床药理学杂志, columnName=研究方法, runingTitle=null, highlight=null, articleAbstract=
目的 建立一种中空纤维离心超滤（HFCF-UF）结合超高效液相色谱法（UPLC）分析人血浆中甲氨蝶呤（MTX）的游离浓度，并用于临床治疗药物监测。
方法 血清样本500 μL经HFCF-UF处理，色谱柱为Waters UPLC BEH C18柱（50 mm×2.1 mm，1.7 μm），流动相为甲醇∶0.05 mol·L-1磷酸缓冲盐（pH=6.2）＝17∶83，流速为0.2 mL·min-1，柱温为30 ℃，检测波长为302 nm。对该方法的专属性、线性关系、定量下限（LLOQ）、精密度、回收率和稳定性进行考察，并用于临床血浆样品的测定。
结果 人血浆中游离MTX在0.05~10.00 μmol·L-1内线性关系良好，y=0.297x+0.001（r2=0.999），MTX游离血药浓度分析的LLOQ为0.05 μmol·L-1，方法回收率为95.77%~100.52%，MTX绝对回收率为84.09%~92.93%，批内、批间相对标准偏差（RSD）均不大于7.0%。该方法成功用于52例用MTX冲击化疗患者体内MTX的游离浓度测定，该52例患者的MTX平均游离血药浓度为0.68 μmol·L-1，最大值为9.32 μmol·L-1，最小值为0.056 μmol·L-1。
结论 本研究所建方法简便、准确、灵敏，适用于临床MTX治疗药物监测。
, authors=董维冲
1, 郭家良
2, 高帅帅
1, 李浩然
1, 李芳婷
1, 蒋晔
3, 张志清
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董维冲（1988-），副主任药师，主要从事治疗药物监测研究
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