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Drug Res (Stuttg) 2016; 66(08): 394-401
DOI: 10.1055/s-0035-1569446
Original Article
© Georg Thieme Verlag KG Stuttgart · New York

Simultaneous Determination of Baicalein and Baicalin in Human Plasma by High Performance Liquid Chromatograph-Tandem Spectrometry and its Application in a Food-Effect Pharmacokinetic Study

H. Pang
1   School of Pharmacy, Shenyang Pharmaceutical University, Shenyang (P.R. China)
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
A. Shi
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
M. Li
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
W. Xue
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
Y. Li
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
G. Cao
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
B. Yan
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
F. Dong
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
W. Xiao
3   StateKey Laboratory of New-tech for Chinese Medicine Pharmaceutical Process, Jiangsu Kanion Pharmaceutical CO.LTD, Lianyungang, Jiangsu (P.R. China)
,
G. He
4   Beijing Key Laboratory of Drug Targets Identification and Drug Screening, Institute of Materia Medica, Chinese Academy of Medical Science and Peking Union Medical College, Beijing (P.R. China)
,
G. Du
4   Beijing Key Laboratory of Drug Targets Identification and Drug Screening, Institute of Materia Medica, Chinese Academy of Medical Science and Peking Union Medical College, Beijing (P.R. China)
,
X. Hu
2   Beijing Key Laboratory of Drug Clinical Risk and Personalized Medication Evaluation, Department of Pharmacy, Beijing Hospital, Beijing (P.R. China)
,
G. Cheng
1   School of Pharmacy, Shenyang Pharmaceutical University, Shenyang (P.R. China)
› Author Affiliations
Further Information

Publication History

received 11 November 2015

accepted 23 February 2016

Publication Date:
29 March 2016 (online)

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Abstract

Background: Baicalein is a flavonoid isolated from skullcap and it is likely to exist in plasma at a low concentration because of the extensive first-pass metabolism in vivo. The aim of our study was to develop and fully validate a sensitive and selective HPLC-MS/MS method for simultaneous determination of baicalein and its main metabolite baicalin (baicalein-7-O-β-glucopyranuronoside) in human plasma.

Materials and methods: Liquid-liquid extraction was used for pretreatment of plasma samples. The mobile phase consisted of aqueous phase A (0.5% formic acid in 3 mM ammonium acetate solution) and organic phase B (methanol-acetonitrile-formic acid, 50:50:0.5, v:v:v). Detection was performed on a triple-quadrupole tandem mass spectrometer using positive electrospray ionization. Quantification was performed by multiple reaction monitoring mode at m/z transitions of 271.1→123.1 for baicalein and 447.1→271.0 for baicalin, respectively.

Results and discussion: The calibration curve was linear over the range of 1~400 ng/mL (r2>0.99) for both baicalein and baicalin. The intra-day and inter-day precision values were below 6.84% for baicalein and 8.56% for baicalin at 3 quality control levels. The mean accuracy was 95.27 ~ 110.56%, 91.82 ~ 105.01% for baicalein and baicalin, respectively. Analytes were stable during sample storage and handling.

Conclusions: The method was proved to be accurate and specific and was applied to a pharmacokinetic study of baicalein in healthy volunteers under both fasted and fed states.

Key words

liquid-liquid extraction - positive electrospray ionization - incurred samples reanalysis
 

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