Simultaneous Quantification of Sodium Ferulate, Salicylic Acid, Cinnarizine and Vitamin B1 in Human Plasma by LC Tandem MS Detection

Abstract

A rapid and simple high performance liquid chromatographic method coupled with tandem mass spectrometry (LC–MS–MS) via electrospray ionization (ESI) has been developed and validated to separate and simultaneously quantify sodium ferulate (SF), salicylic acid (SA), cinnarizine (CIN) and vitamin B1 (VB1) in human plasma. Gemfibrozil (GEM) was used as the internal standard (IS) for SF and SA, whereas lomerizine (LOM) was used as the IS for CIN and VB1. The plasma samples were prepared by one-step protein precipitation followed by an isocratic elution with 10 mM ammonium acetate buffer (pH = 5.0): acetonitrile (35:65, v/v,) on an Agilent Zorbax SB-CN column (150 mm × 2.0 mm ID, 5 μm). The precursor and product ions of these drugs were monitored on a triple quadrupole mass spectrometer, operating in the selected reaction monitoring mode (SRM) with polarity switch, in the negative-ion mode for SF, SA and GEM, in the positive-ion mode for CIN, VB1 and LOM. The method was validated over the concentration range of 1.5–1,000 ng mL−1 for SF, 20–5,000 ng mL−1 for SA, 2–500 ng mL−1 for CIN, 1–30 ng mL−1 for VB1. The intra- and inter-batch precisions were less than 15% of the relative standard deviation. The recoveries for analytes and IS achieved from spiked plasma samples were consistent and reproducible. The validated LC–MS–MS method has been successfully applied to the pharmacokinetic study of sodium ferulate and aspirin capsule in healthy volunteers.