Determination of pilsicainide in human plasma and urine by LC-MS/MS / 中国药学杂志

ABSTRACT

OBJECTIVE: To develop a sensitive and specific LC-MS/MS method for the determination of pilsicainide in human plasma and urine. METHODS: The samples were processed by LLE(liquid-liquid extraction), acetonitrile-ammonium acetate(0.1‰ formic acid)-water was used as the mobile phase with isocratic elution(2537.537.5 in plasma, 35659 in u-rine), and separation was carried out on Welch Material Ultimate AQ-C18 column(2.100 × 100 mm, 3.5 μm), setting the flow rate as 0.35 mL · min-1, the column temperature at 25°C. The injection volume was 5 μL. ESI under positive ion mode and multiple reaction monitoring scan(MRM) were used for quantitative analysis with m/z 213.4 → 110.2 for pilsicainide and m/z 287.4 → 110.2 for internal standard, methyl-pilsicainide. RESULTS: The linear ranges of the calibration curves for pilsicainide were 1-1200 μg · L-1 for plasma and 1-150 mg · L-1 for urine. The limitation of detection were 1 μg · L-1 for plasma and 1 mg · L-1 for urine. The correlation coefficient was between 0.9962 and 0.9991. The extraction recoveries, matrix effects, and intra-/inter-assay precisions all met the requirements of pharmacokinetic studies. This approach was applied to determine pilsicainide concentrations in human plasma and urine in a clinical pharmacokinetic research. CONCLUSION: This approach possesses convenience, accuracy, high sensitivity and good reproducibility, which can meet the requirements of pharmacokinetic studies.