LC-MS/MS method for quantification of methylergonovine in human plasma and its application in pharmacokinetic study of methylergonovine maleate tablets
10.13699/j.cnki.1001-6821.2019.07.025
- VernacularTitle:LC-MS/MS法测定人血浆中甲麦角新碱浓度及药代动力学研究
- Author:
Yang LI
1
;
Hui-Hong QI
;
Hong-Xian PANG
;
Wen-Yuan QI
;
Ai-Xin SHI
Author Information
1. 北京医院 国家老年医学中心
- Keywords:
methylergonovine;
liquid chromatograph-tandem mass spectrometer;
pharmacokinetics
- From:
The Chinese Journal of Clinical Pharmacology
2019;35(7):686-689
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a LC-MS/MS method for pharmacokinetics study of methylergonovine in healthy Chinese volunteers after single and multiple-dose administration of methylergonovine maleate tablets. Methods 6-hydroxyflavone was used as internal standard.The separation was achieved on a Waters Xterra C18 (2. 1 mm × 100 mm, 3. 5 μm) with a mobile phase consisting of 0. 05％ ammonium acetate and methanol-acetonitrile (80:20) solution. At a flow rate of 0. 3 m L·min-1 within 12 min. Methylergonovine and 6-hydroxyflavone were measured by ESI in positive electron mode using multiple reaction monitoring (MRM) . The extracted ions monitored following MRM transitions were m/z 340. 3 →223. 2 for methylergonovine and m/z 239. 2 →129. 1 for 6-hydroxyflavone. Plasma samples were pretreated by liquid-liquid extraction. Results The calibration curve was linear within the range of 0. 1-20. 0 ng·m L-1. The Lower limit of quantitation was 0. 1 ng·m L-1 and CV％ of intra-and inter-day were less than 15％. The plasma samples were stable at room temperature (25 ℃) for 4 h, at-70℃ for 4 months and during three freeze-thaw cycles. There was no accumulationafter ultiple-dose of methylergonovine maleate tablets.Conclusion The method was proved to be accurate and sensitive suitable for the pharmacokinetics of methylergonovine in volunteers after oral administration of 0. 125, 0. 25, 0. 5 mg methylergonovine maleate tablets.
