Chuẩn hóa nhận diện và xác định độ tinh khiết hóa phóng xạ bằng HPLC đối với dược chất phóng xạ 18F-NaF được điều chế tại bệnh viện Trung ương Quân đội 108

Validation of the method to use HPLC for determination for identity and radiochemical purity of 18F-NaF radiopharmaceutical produced at 108 Hospital

SUMMARY

Objective: This study was aimed to standardize the method of determining identity and radiochemical purity of 18F-NaF according to European Pharmacopoeia and to adapt it to the quality control system of the Cyclotron center at 108 Hospital.

Material and Methods: Agilent 1200 HPLC connected to Carbopac PA10 collumn from Dionex, UV detector and radioactive detector, injector with a multiport valve and a 20μL calibrated loop; Satorius analytical balance with accuracy 0.001g; NaOH from Merk; standard NaF from ABX; ultrapure water from Millipore Milli-Q system. The identification of 18F-NaF is done on HPLC by comparing the retention time (tR) by the radiochemical detector, and tR of the NaF reference UV detector. We determined the difference between the detectors expressed in time and then correct the tR of 18F-NaF peak. After this, we determined the difference between corected tR of 18F-NaF and tR of NaF expressed in minute and the percentage deviation of the corrected value of 18F-NaF from the reference NaF.

Results: The results met all requirements in the ICH Q2(R1) guidelines. The calibration curve (0,125-5 mg/ml NaF) had R2 for peak area and height againt concentration are 0.998 and 0.997 respectively. The precision with sample of 1,95 mg/ml NaF has R2 < 5%. The acuracy has the percent recovery from 98.97-100.21% with R2> 0,99 and RSD < 2%. The robustness has RSD = 0.31% < 2%. Validaion of identity and radiochemical purity test of 8F-NaF showed that the deviation of retention time NaF and 18F-NaF was 0,12- 0,52%; the linearity of the radiochemical purity test had R2 >0,99; the precision of the HPLC method was expressed in results of 5 times of measurement of a 18F-NaF sample, that gave RSD = 0,29%.

Conclusion: The results of the study show that the HPLC 1200 can give an accuracy and reliability for analysis of radiochemical purity and identity tests of 18F-NaF that is under studying at 108 Hospital.

Key words: NaF, 18F-NaF, HPLC, radiopharmaceutical purity