Determination of fexofenadine in human plasma using 96-well solid phase extraction and HPLC with tandem mass spectrometric detection.
Determination of fexofenadine in human plasma using 96-well solid phase extraction and HPLC with tandem mass spectrometric detection.
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使用 96 孔固相萃取和串联质谱检测 HPLC 测定人血浆中的非索非那定。
DOI：
10.1016/j.jpba.2004.02.016
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发表时间：
2004
影响因子：
3.4
通讯作者：
B. K. Matuszewski
中科院分区：
文献类型：
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作者：
I. Fu;E. Woolf;B. K. Matuszewski
描述了一种快速、灵敏的HPLC-MS/MS方法，利用大气压化学电离法测定人血浆中的非索非那定。氘代类似物d 6-非索非那定用作内标（IS）。使用96孔固相萃取用含有沃茨Oasis HLB吸附剂的板制备血浆样品。在Restek Ultra IBD色谱柱（3.2 mm ×50 mm，3μm）上，使用由90%乙腈和10% 10 mM乙酸铵缓冲液和0.1%甲酸组成的移动的流动相对分析物进行色谱分析。分析物的定量是基于非索非那定（m/z 502→466）和d 6-非索非那定（m/z 508→472）的前体-产物离子对的多反应监测响应。根据对0.5 ml血浆等分试样的分析，在1- 200 ng/ml浓度范围内对该测定法进行了验证。日内测定准确度为标称值的97 - 102%，而标准曲线上所有点的日内精密度均优于3.5% CV。在标准曲线范围内，分析物提取回收率优于70%。发现该方法适用于分析60 mg非索非那定单次给药后24小时获得的人血浆样品。
A fast and sensitive HPLC–MS/MS method, utilizing atmospheric pressure chemical ionization, for the determination of fexofenadine in human plasma is described. A deuterated analog, d6-fexofenadine is used as the internal standard (IS). Plasma samples are prepared using 96-well solid phase extraction with plates containing Waters Oasis HLB sorbent. The analytes are chromatographed on a Restek Ultra IBD column (3.2 mm ×50 mm, 3μm) using a mobile phase consisting of a mixture of 90% acetonitrile and 10% 10mM ammonium acetate buffer and 0.1% formic acid. Quantitation of the analyte is based on the response from the multiple reaction monitoring of the precursor to product ion pairs for fexofenadine (m/z 502→466) and d6-fexofenadine (m/z 508→472). The assay has been validated over the concentration range of 1–200ng/ml based on the analysis of 0.5ml aliquots of plasma. Within-day assay accuracy was between 97 and 102% of nominal, while within-day precision was better than 3.5% CV at all points on the standard curve. Analyte extraction recovery was better than 70% over the range of the standard curve. The method was found to be suitable for the analysis of human plasma samples obtained 24h following the administration of a single 60mg dose of fexofenadine.
DOI：
--
发表时间：
1999-08
期刊：
Drug metabolism and disposition: the biological fate of chemicals
影响因子：
--
作者：
M. Cvetkovic;B. Leake;M. Fromm;G. Wilkinson;R. Kim
通讯作者：
M. Cvetkovic;B. Leake;M. Fromm;G. Wilkinson;R. Kim