A liquid chromatography mass spectrometry assay for determination of PD168393, a specific and irreversible inhibitor of erbB membrane tyrosine kinases, in rat serum.
A liquid chromatography mass spectrometry assay for determination of PD168393, a specific and irreversible inhibitor of erbB membrane tyrosine kinases, in rat serum.
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DOI：
10.1016/j.jchromb.2008.10.046
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发表时间：
2008-12-15
期刊：
影响因子：
--
通讯作者：
Carroll SL
中科院分区：
文献类型：
--
作者：
Prasain JK;Arabshahi A;Moore R;Barnes S;Carroll SL
首次开发并验证了使用大气压化学电离源（APCI）的快速、灵敏和简单的液相色谱/串联质谱（LC-MS/MS）方法，用于定量测定大鼠血清中的PD 168393。血清样品用甲醇预处理用于蛋白沉淀。色谱柱为C5柱（250 × 2.0 mm i.d），用0.1%甲酸预平衡。在多反应监测模式下调谐串联质谱仪，以使用正离子模式监测PD 168393的m/z跃迁369/313和内标物三唑仑的m/z跃迁343/308。MS/MS响应在2- 5，000 ng/mL浓度范围内呈线性，定量下限（LLQ）为2 ng/mL。在最低质量控制（4 ng/mL）下，PD 168393的日内和日间精密度（CV%）小于10%，准确度在92- 111%之间。验证的方法可用于筛选和优化过程的大部分或所有阶段，用于未来药代动力学研究的方法验证。
For the first time, a rapid, sensitive and simple liquid chromatography/tandem mass spectrometry (LC-MS/MS) method using an atmospheric pressure chemical ionization source (APCI) for the quantification of PD168393 in rat serum was developed and validated. Serum samples were pretreated with methanol for protein precipitation. The chromatographic separation was performed on a Jupiter-C5 column (250 × 2.0 mm i.d) pre-equilibrated with 0.1% formic acid. The tandem mass spectrometer was tuned in the multiple reaction monitoring mode to monitor the m/z transitions 369/313 for PD168393 and m/z 343/308 for the internal standard triazolam, using positive ion mode. The MS/MS response was linear over the concentration range from 2–5,000 ng/mL, with a lower limit of quantification (LLQ) of 2 ng/mL. At the lowest quality control (4 ng/mL), the intra- and inter-day precisions (CV%) for PD168393 were less than 10% and the accuracies were between 92–111 %. The validated method can be used in most or all stages of the screening and optimizing process for future method validation of pharmacokinetic studies.
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影响因子：
13.5
作者：
Fry, DW
通讯作者：
Fry, DW
DOI：
10.1081/jlc-100101455
发表时间：
2000-01-01
影响因子：
1.3
作者：
Rosing, H;Man, WY;Beijnen, JH
通讯作者：
Beijnen, JH
DOI：
10.1073/pnas.95.20.12022
发表时间：
1998-09-29
影响因子：
11.1
作者：
Fry, DW;Bridges, AJ;Dobrusin, EM
通讯作者：
Dobrusin, EM
影响因子：
7.4
作者：
Matuszewski, BK;Constanzer, ML;Chavez-Eng, CM
通讯作者：
Chavez-Eng, CM
DOI：
10.1016/j.jpba.2004.03.020
发表时间：
2004-09-03
影响因子：
3.4
作者：
Chavez-Eng, CM;Constanzer, ML;Matuszewski, BK
通讯作者：
Matuszewski, BK