Determination the concentraiton of nifedipine and its metabolite dehydronifedipine in rat plasm by LC-MS/MS
10.13699/j.cnki.1001-6821.2017.23.027
- VernacularTitle:LC-MS/MS法测定大鼠血浆中硝苯地平及其代谢物氧化硝苯地平的浓度
- Author:
Nan HU
1
;
Xiao-Yu LU
;
Di ZHAO
;
Li-Ying WANG
;
Su-Lan ZOU
Author Information
1. 常州市第一人民医院药剂科,江苏常州213003
- Keywords:
LC-MS/MS;
nifedipine;
dehydronifedipine;
plasma concentration
- From:
The Chinese Journal of Clinical Pharmacology
2017;33(23):2420-2423
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a high performance liquid chromatography-tandam mass spectrometry (LC-MS/MS) method for determining the concentration of nifedipine and its main metabolite dehydronifedipine in rat plasma.Methods The nifedipine,dehydronifedipine and internal standard diazepam were extracted from plasma with protein precipitation by acetonitrile,then the supernatant was separated on SHIMADZU Shim-pack VP-ODS C18 column(2.0 mm ± 150 mm,5 μm),and eluted by acetonitrile-water (containing 0.1％ formic acid) with a gradient elution.The flow rate was 0.35 mL · min-1 Detection of the analytes were achieved using positive ion electrospray ionization in the multiple reaction monitoring mode.The MS/MS ion transitions monitored were m/z 347.2/315.3,345.1/268.1,and 285.3/154.2 for nifedipine,dehydronifedipine and diazepam respectively.Results Nifedipine had a good linear relationship in the range of 2-1000 ng · mL-1 with the calibration curve y =3.07 × 10-2x + 8.42 × 10-2 (r =0.998 9),and the lowest of quantification was 2 ng · mL-1 Dehydronifedipine had a good linear relationship in the range of 2-200 ng · mL-1 with the calibration curve y =4.53 × 10-2x + 2.28 × 10-2 (r =0.996 6),and the lowest of quantification was 2 ng· mL-1.Intra-day and inter-day relative standard deviations (RSDs) of blood samples were less than 15％,and the absolute recovery in plasma was above 90％.Conclusion The established method in this study was simple,rapid,sensitive,specific,and suitable for the determination of nifedipine and dehydronifedipine in rat plasma.
