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J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 1;1061-1062:123-127. doi: 10.1016/j.jchromb.2017.07.011. Epub 2017 Jul 8.

Development of a LC-MS/MS method for the determination of CKD-712 in rat plasma: Application to a pharmacokinetic study in rats.

Author information

1
Department of Pharmacy, National University of Singapore, Singapore.
2
College of Pharmacy, Chungnam National University, Daejeon, Republic of Korea.
3
Korea Institute of Toxicology, Daejeon, Republic of Korea.
4
Graduate School of New Drug Discovery and Development, Chungnam National University, Daejeon, Republic of Korea.
5
Korea Institute of Toxicology, Daejeon, Republic of Korea. Electronic address: jhl@kitox.re.kr.

Abstract

CKD-712 is a potential treatment for sepsis, as it exhibits protective effects against lipopolysaccharide-mediated platelet aggregation, inducible nitric oxide synthase expression, and cecum-ligation puncture-induced septic mortality in mice. In this study, we develop a rapid and sensitive LC-MS/MS method for determining CKD-712 in rat plasma. CKD-712 and papaverine hydrochloride (an internal standard) were analyzed using an LC-MS/MS system consisting of an Agilent HPLC system (HP-1100) equipped with an Atlantis HILIC Silica (2.1×50mm, 3μm) column and a API 4000 (Applied Biosystems/MDS Sciex, USA) in a positive ESI mode. We utilized multiple reaction monitoring (MRM) at m/z transitions of 306.2-164.0 to analyze CKD-712, and 340.3-202.1 m/z for IS, with a mobile phase of acetonitrile (0.025% trifluoroacetic acid):20mM ammonium acetate (94:6, v/v) at a flow rate of 0.25mL/min. The lower limit of quantification (LLOQ) was 5ng/mL, with a linearity ranging from 5 to 1000ng/mL (r>0.999). Validation parameters including specificity, precision, accuracy, matrix effect, recovery, dilution effect and stability results were well within acceptance criteria, and applied successfully on a pharmacokinetic study in rats.

KEYWORDS:

CKD-712; LC/MS/MS; Method validation; Pharmacokinetics; Rat plasma

PMID:
28734159
DOI:
10.1016/j.jchromb.2017.07.011
[Indexed for MEDLINE]

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