title: A method for analysis of wilfordmine in human plasma by liquid chromatography coupled with ion trap mass spectrometry.
abstract: A simple and rapid liquid chromatography-ion trap mass spectrometric (LC-IT/MS) method has been developed and validated for quantification of wilfordmine in human plasma. After the protein precipitation was carried out by acetonitrile and the solution was cleaned by solid-phase extraction, the chromatographic separation was performed on a Zorbax Plus RRHD C18 column by using a mixture of acetonitrile and 10.0 mmol/L ammonium acetate solution (70:30, v/v) as the mobile phase at a flow rate of 0.7 mL/min. Detection was performed on an atmospheric-pressure chemical ionization source in the positive multiple reaction monitoring mode using aconitine as an internal standard (IS) with transitions of m/z 806→710 for wilfordmine, and 646→586 for IS, respectively. The obtained calibration curve was linear (r = 0.9992) over the concentration range of 0.5-100.0 μg/L with a lower limit of quantification of 0.5 μg/L in plasma. The intra- and interday relative standard deviations were <7.0 and 12.3%, respectively. The recoveries were between 86.0 and 97.0%. The proposed method was found to be applicable to clinical studies.
authors.affiliation: Public Health Department of Medical School, Zhejiang Provincial Key Laboratory of Pathological and Physiological Technology, Ningbo University, Ningbo 315211, China.
authors.forename: Lixin
authors.initials: L
authors.lastname: Zhou
authors.affiliation: Public Health Department of Medical School, Zhejiang Provincial Key Laboratory of Pathological and Physiological Technology, Ningbo University, Ningbo 315211, China.
authors.forename: Hao
authors.initials: H
authors.lastname: Zhu
authors.affiliation: School of Food and Medicine, Zhejiang Ocean University, Zhoushan 316004, China.
authors.forename: Xiaokun
authors.initials: X
authors.lastname: Ouyang
authors.affiliation: Public Health Department of Medical School, Zhejiang Provincial Key Laboratory of Pathological and Physiological Technology, Ningbo University, Ningbo 315211, China.
authors.forename: Jinshun
authors.initials: J
authors.lastname: Zhao
authors.affiliation: Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China chenxhnb@163.com.
authors.forename: Xiaohong
authors.initials: X
authors.lastname: Chen
mesh_terms: D000470:Alkaloids / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004365:Drugs, Chinese Herbal / Q000032:analysis*; D006801:Humans; D013058:Mass Spectrometry / Q000379:methods*
chemical_list: D000470:Alkaloids; D004365:Drugs, Chinese Herbal