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Simultaneous determination of dipyridamole and salicylic acid in human plasma by high performance liquid chromatography-mass spectrometry

2007; Wiley; Volume: 22; Issue: 2 Linguagem: Inglês

10.1002/bmc.909

1099-0801

Na Wang, Fengguo Xu, Zunjian Zhang, Cheng Yong Yang, Xiuhong Sun, Jin‐Heng Li,

Cerebrovascular and Carotid Artery Diseases

Abstract A sensitive, rapid and simple high‐performance liquid chromatography–electrospray ionization–mass spectrometry (HPLC‐ESI‐MS) method for simultaneous determination of dipyridamole and salicylic acid in human plasma has been developed and validated. After the addition of diazepam and rosiglitazone as internal standard (IS), plasma samples were prepared by liquid–liquid extraction followed by an isocratic elution with methanol:2 m m ammonium acetate buffer (pH 4.25; 70/30, v/v) on a Shimadzu VP‐ODS C 18 column (5 µm, 150 × 2.0 mm I.D.). Detection was performed on a quadrupole mass spectrometer with ESI interface operating in the positive‐ion mode for dipyridamole and negative‐ion mode for salicylic acid. Calibration curves were linear ( r 2 > 0.99) over the concentration range 10–2500 ng/mL for dipyridamole and 30–4000 ng/mL for salicylic acid with acceptable accuracy and precision, respectively. The intra‐ and inter‐batch precisions were less than 15% of the relative standard deviation. The limits of detection of dipyridamole and salicylic acid were 1 and 15 ng/mL, respectively. The validated HPLC‐ESI‐MS method was successfully applied to a preliminary pharmacokinetic study of fixed‐dose combination of sustained‐release dipyridamole/aspirin in Chinese healthy male volunteers. Copyright © 2007 John Wiley & Sons, Ltd.