Determination of propylthiouracil in human plasma by UPLC-MS/MS / 药学实践杂志

ABSTRACT

Objective To establish a method for the determination of propylthiouracil in human plasma by UPLC-MS/MS and provide methodological basis for therapeutic drug monitoring (TDM) and bioequivalence test (BE) in clinical. Methods The chromatographic separation was performed on an Agilent SB-C18 column (4.6 mm×150 mm, 5 μm), the mobile phase was methanol and water containing 0.1% formic acid (80∶20, V/V), isocratic elution. MS condition was optimized in the positive ion detection mode by multiple reaction monitoring (MRM), along with the Agilent JetStream electrospray source interface (AJS-ESI). The precursors to the product ion transitions were m/z 171.1→112.1 for propylthiouracil and m/z 176.1→117.0 for the internal standard (IS). Results The calibration curve was linear in the range of 10−5 000 ng/ml for propylthiouracil in human plasma, r=0.999 3. The intra-day and inter-day precision and accuracy were good (RSD<10%，RE<±10%). The matrix effect of different concentrations was less than 110% and the coefficient of variation was less than 5%. The average recovery of different concentrations was 101.60%−113.56%, which conformed with the requirement of methodological validation. Conclusion The method is rapid, sensitive and accurate, which can be used for the determination of propylthiouracil in human plasma.