title: Quantitative determination of dipyridamole in human plasma by high-performance liquid chromatography-tandem mass spectrometry and its application to a pharmacokinetic study.
abstract: Dipyridamole is a classic platelet inhibitor which has been a key medicine in clinical therapy of thrombosis and cerebrovascular disease. A rapid, selective and convenient method using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for determination of dipyridamole in human plasma. After protein precipitation of 200 microL plasma with methanol, dipyridamole and diazepam (internal standard) were chromatographed on an Ultimate XB-C(18) (50 x 2.1 mm i.d, 3 microm) column with the mobile phase consisting of methanol-ammonium acetate (5 mM; 80 : 20, v/v) at a flow rate of 0.25 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring mode via positive eletrospray ionization source (ESI(+)). The retention times of dipyridamole and diazepam were 1.4 and 1.2 min, respectively. The method was validated over a concentration range of 0.0180-4.50 microg/mL (r(2) > or = 0.99) with a lower limit of quantitation (LLOQ) of 0.0180 microg/mL for dipyridamole. The intra- and inter-day precisions (RSD) of the assay at all three QC levels were 1.6-12.7% with an accuracy (RE) of -4.3-1.9%, which meets the requirements of the FDA guidance. The HPLC-MS/MS method herein described was proved to be suitable for pharmacokinetic study of sustained-release dipyridamole tablet in volunteers after oral administration.
authors.affiliation: Department of Analytical Chemistry, Shenyang Pharmaceutical University, People's Republic of China.
authors.forename: Ting
authors.initials: T
authors.lastname: Qin
authors.forename: Feng
authors.initials: F
authors.lastname: Qin
authors.forename: Ning
authors.initials: N
authors.lastname: Li
authors.forename: Shan
authors.initials: S
authors.lastname: Lu
authors.forename: Wei
authors.initials: W
authors.lastname: Liu
authors.forename: Famei
authors.initials: F
authors.lastname: Li
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000191:economics / Q000379:methods*; D004176:Dipyridamole / Q000097:blood*; D006801:Humans; D057230:Limit of Detection; D008297:Male; D010975:Platelet Aggregation Inhibitors / Q000097:blood*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000191:economics / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods*; D013997:Time Factors
chemical_list: D010975:Platelet Aggregation Inhibitors; D004176:Dipyridamole