Validation of the FDG (18F) radiochemical purity assay by thin layer chromatography

Abstract

All methodologies utilized in radiopharmaceutical industry should be validated in order to prove that they meet the requirements of analytical applications, ensuring the reliability of the results. At a radiopharmaceutical industry there is one challenge aspect: sometimes it is not possible use a stable standard to perform the validation analysis. In order to overcome this difficulty, the objective of this study was to suggest a validation protocol for these methodologies, based on the recommendations of RE n° 899/Agência Nacional de Vigilância Sanitária (ANVISA), and prove its efficiency, performing the radiochemical purity validation test of FDG (18F), by TLC. To obtain the calibration curve, we suggested that the theoretical activity values should be determined using a dose calibrator, simultaneously of each analysis performed by TLC, for 5 hours. The method was linear (R2 of 0.996), precise (CV% <5%) and accurate (96.85% < accuracy < 102.56%). In relation to the robustness test, our experiments evaluated the influence of the distance travelled by mobile phase, variations at mobile phase concentration and type of chromatographic plate (silica gel on glass or aluminium plates). The detection and quantification limits were determined (321.9 and 1065.6 kBq, respectively). As expected, this methodology was nonspecific, showing a slight spot corresponding to the FDM. The proposed protocol was efficient and the methodology tested was effective to determine the radiochemical purity of FDG (18F), in accordance to the limits recommended by ANVISA.