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Development and validation of a highly sensitive LC-MS/MS method for the determination of acacetin in human plasma and its application to a protein binding study

Title
Development and validation of a highly sensitive LC-MS/MS method for the determination of acacetin in human plasma and its application to a protein binding study
Author
송충길
Keywords
Acacetin; LC-MS/MS; Human plasma; Protein binding
Issue Date
2016-02
Publisher
PHARMACEUTICAL SOC KOREA
Citation
ARCHIVES OF PHARMACAL RESEARCH, v. 39, NO 2, Page. 213-220
Abstract
A highly sensitive bioanalytical method for the quantification of acacetin in human plasma was developed and comprehensively validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A minimal volume of human plasma sample (20 mu L) was prepared by simple deproteinization with 80 mu L of acetonitrile. Chromatographic separation was performed using Kinetex C-18 column with an isocratic mobile phase consisting of water and acetonitrile (20:80, v/v) containing 0.1 % formic acid at a flow rate of 0.3 mL/min over a total run time of 2.0 min. Mass spectrometric detection was performed using multiple reaction-monitoring modes at the mass/charge transitions m/z 285.22 -˃ 242.17 for acacetin and m/z 277.59 -˃ 175.04 for chlorpropamide (internal standard). The calibration curve was linear over the range of 0.1-500 ng/mL with a lower limit of quantitation of 0.1 ng/mL. The coefficients of variation for both intra- and inter-day validation were less than 11.9 %, and the intra- and inter-day accuracy ranged from 96.8 to 108 %. Mean recovery of acacetin in human plasma was within the range of 91.5-95.6 %. This validated LC-MS/MS method was successfully applied to a human plasma protein binding study that indicated extensive and concentration-independent protein binding of acacetin in human plasma.
URI
https://link.springer.com/article/10.1007%2Fs12272-015-0697-1http://hdl.handle.net/20.500.11754/34146
ISSN
0253-6269; 1976-3786
DOI
10.1007/s12272-015-0697-1
Appears in Collections:
RESEARCH INSTITUTE[S](부설연구소) > ETC
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