Determination of Valproate Acid in Human Plasma by UFLC-MS/MS / 中国药师

ABSTRACT

To establish a UFLC-MS/MS method for the determination of valproate acid in human plasma. Methods:The sample was precipitated by methanol. The analysis of valproate acid and diclofenac sodium ( internal standard) was carried out on a Shim-pack XR-ODS II C18 column (2. 0 × 75 mm,2. 2 μm). Gradient elution was adopted with acetonitrile and water (containing 5 mmol·L-1 ammonium acetate) at a flow rate of 0. 3 ml·min-1. The detection was performed with multiple reactions monitoring (MRM) using nega-tive electrospray ionization (ESI) at m/z 142. 8→142. 8 for valproate acid and m/z 294. 0→249. 8 for diclofenac sodium. Results: The calibration curve of valproate acid was linear over the range of 8.4-168.0 μg·ml-1(r=0.997 5). Inter- and intra-day RSDs were less than 15%, and the analysis was proven to be stable. Totally 30 samples determined by EMIT were assayed by the method. And the results of the two methods analyzed by independent t-test showed no statistical significance. Conclusion:The method is rapid,sensitive and spe-cific,which can be applied in the determination of valproate acid in human plasma.