RESUMO
OBJECTIVE: To establish an analytical method for determination of mesaconine in rat plasma or dialysate, and study the rat plasma protein binding rate of mesaconine. METHODS: The equilibrium dialysis method was applied to determine the in vitro plasma protein binding rate of mesaconine. A UPLC-MS/MS method was established to determine mesaconine in the intra- and extradialysis samples and then the plasma protein binding rate was calculated. RESULTS: The specificity of the established UPLC-MS/MS method was very good. The calibration curve of mesaconine had good linearity over the range of 0.156 3 - 10 μg•mL-1. The intra-day and inter-day precisions and recovery met the requirements of methodology. The plasma protein binding rates of mesaconine were 18.73%, 20.20%, 26.59%, and 23.68% at the concentrations of 0.2, 0.5, 2.0, and 5.0 μg•mL-1, respectively. CONCLUSION: The method is simple, accurate and sensitive, and can meet the requirement for analysis method of biological samples. Mesaconine has a low rat plasma protein binding rate.
RESUMO
OBJECTIVE: To establish an HPLC-ELSD method for determination of mesaconine. METHODS: Gemini C18 110A column (4.6 mm×150 mm, 5 μm) was adopted with the mobile phase consisting of methanol-0.1%TFA (25:75) at the flow rate of 0.6 mL·min-1. The detector was Alltech ELSD 2000ES, with the drift tube temperature of 90℃ and the airflow velocity of 2.3 L·min-1. RESULTS: Under this conditions, mesaconine and the related substances were well separated. The linear range of mesaconine was 0.40-0.60 mg·mL-1 (r=0.9996). RSD of injection precision and repeatability test were 0.04% (n=5) and 0.7% (n=6), the intra day and inter day precision RSD were 0.4% and 0.6%, respectively. The average recovery was 101. 0% (RSD=1.1%, n=9). CONCLUSION: The established method was specific, simple, accurate, and suitable for determination of mesaconine.