Validation of routine analytical method for injectable cyclosporine preparation control using HPLC-FIA assay.

Objective: The aim of this study is to validate a new HPLC-FIA method for routine analytical control of cyclosporine injectable preparations and to evaluate the routine analytical control with this technic.

Material And Methods: Cyclosporine dosage was carried out by the HPLC-FIA method. The column was replaced by a PEEK (polyetheretherketone) loop tubing. The mobile phase consisted of ultrapure water. The injection volume was 1μL with a flow rate of 1mL/min. All determinations were performed at 35°C. The detection was carried out at 210nm. The accuracy profile method was used to validate the HPLC-FIA assay of cyclosporine. Routine control was applied for each cyclosporine preparation using the HPLC-FIA developed method. An acceptance limit of ±10% of the theoretical concentration has been set for the conformity of the preparation.

Results: The accuracy profile shows the validity of our method for the dosage of cyclosporine in the concentration range studied (0.5-2.5mg/mL) with good linearity (correlation coefficient>0.999), high precision (the relative standard deviation [RSD] values, for both repeatability and intermediate precision, were<3%) and acceptable trueness (the relative biases were found<2%). In our study, 220 injectable cyclosporine preparations were analyzed: 85% were compliant. All analyzes were conform after a second standardized homogenization of 10 shakes.

Conclusions: The proposed HPLC-FIA method is a reliable, fast, simple, precise method that can be easily used for the routine quality control of cyclosporine injectable preparations.