Determination of talinolol in human plasma using automated on-line solid phase extraction combined with atmospheric pressure chemical ionization tandem mass spectrometry

被引:13
作者
Bourgogne, E [1 ]
Grivet, C [1 ]
Hopfgartner, G [1 ]
机构
[1] Univ Geneva, Lab Pharmaceut Analyt Chem, Sch Pharm, CH-1211 Geneva, Switzerland
来源
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2005年 / 820卷 / 01期
关键词
talinolol; quantitative analysis; column-switching; LC-MS/MS;
D O I
10.1016/j.jchromb.2005.03.007
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A specific LC-MS/MS assay was developed for the automated determination of talinolol in human plasma, using on-line solid phase extraction system (prospekt 2) combined with atmospheric pressure chemical ionization (APCI) tandem mass spectrometry. The method involved simple precipitation of plasma proteins with perchloric acid (contained propranolol) as the internal standard (IS) and injection of the supernatant onto a C-8 End Capped (10 turn x 2 mm) cartridge without any evaporation step. Using the back-flush mode, the analytes were transferred onto an analytical column (XTerra C-18, 50 mm x 4.6 mm) for chromatographic separation and mass spectrometry detection. One of the particularities of the assay is that the SPE cartridge is used as a column switching device and not as an SPE cartridge. Therefore, the same SPE cartridge could be used more than 28 times, significantly reducing the analysis cost. APCI ionization was selected to overcome any potential matrix suppression effects because the analyte and IS co-eluted. The mean precision and accuracy in the concentration range 2.5-200 ng/mL was found to be 103% and 7.4%, respectively. The data was assessed from QC samples during the validation phase of the assay. The lower limit of quantification was 2.5 ng/mL, using a 250 mu L plasma aliquot. The LC-MS/MS method provided the requisite selectivity, sensitivity, robustness accuracy and precision to assess pharmacokinetics of the compound in several hundred human plasma samples. (c) 2005 Elsevier B.V. All rights reserved.
引用
收藏
页码:103 / 110
页数:8
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