Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
10553548 | Journal of Pharmaceutical and Biomedical Analysis | 2011 | 7 Pages |
Abstract
We developed a sensitive, selective and accurate method based on liquid chromatography with tandem mass spectrometry (LC-MS/MS) to determine N-terminal thymosin-β peptides of Ac-SDKP and Ac-ADKP in human plasma samples. Quantification of Ac-SDKP and Ac-ADKP was performed using solid phase extraction (SPE) based on C18, reversed phase LC separation, and stable isotope dilution electrospray ionization-MS/MS in multiple reaction-monitoring (MRM) mode. The Ac-SDKP-13C6, 15N2 and Ac-ADKP-d7 were synthesized for the internal standards. These MRM monitoring ions were m/z 488 â 129 (quantitative ion)/226 for Ac-SDKP, m/z 496 â 137 for Ac-SDKP-13C6, 15N2, m/z 472 â 129 (quantitative ion)/226 for Ac-ADKP, and m/z 479 â 129 for Ac-ADKP-d7, respectively. Lower limit of quantitation (LLOQ) of Ac-SDKP and Ac-ADKP was 0.1 ng/mL in human plasma. Recovery values were ranged from 94.7% to 106.3% for inter- (RSD: 0.6-3.5%) and intra- (RSD: 0.4-4.9%) day assays. Plasma Ac-SDKP levels were significantly higher in hemodialyzed subjects treated with angiotensin-converting enzyme inhibitors of enalapril (27.3 ± 24.6 ng/mL, n = 10) and trandolapril (12.3 ± 16.9 ng/mL, n = 18) than healthy (0.4 ± 0.2 ng/mL, n = 7) and hemodialyzed subjects (0.6 ± 0.2 ng/mL, n = 34). This analytical method would be useful to measure N-terminal thymosin-β peptides in human plasma for the clinical study.
Keywords
Related Topics
Physical Sciences and Engineering
Chemistry
Analytical Chemistry
Authors
Koichi Inoue, Ayaka Ikemura, Yoshinari Tsuruta, Kazuki Watanabe, Kaname Tsutsumiuchi, Tomoaki Hino, Hisao Oka,