Table 3 Tests, methods and acceptance criteria for the quality control of [18F]DPA-714
From: Optimised GMP-compliant production of [18F]DPA-714 on the Trasis AllinOne module
Test | Method | Specifications at release |
|---|---|---|
At product release | ||
Appearance | Visual inspection | Clear and colourless, free from visible particles |
(Radio)chemical identity of [18F]DPA-714 | HPLC (UV, gamma ray detectors) | [18F]DPA-714 peak in the radiochromatogram is consistent with the retention time of the reference standard to the nearest ±0.5 min, taking detector delay into account |
Radionuclidic identity of fluorine-18 | Gamma ray spectrometer | Energy of the principal gamma photon is 511 ±10 keV, possibility of sum peak at 1022 ±20 keV |
Radionuclidic identity of fluorine-18 (half-life measurement) | Ionisation chamber | 1.75-1.92 h |
Radionuclidic purity of fluorine-18 | Gamma ray spectometer | Fluorine-18 ≥99.9% of total activity |
Radiochemical identity of [18F]DPA-714 | HPLC (gamma ray detector) | Retention time of [18F]DPA-714 consistent with retention time of DPA-714 (±0.5 min) |
Radiochemical purity of [18F]DPA-714 | HPLC (gamma ray detector) | ≥95% of total fluorine-18 activity |
pH | pH strip | 4.5-8.5 |
Chemical concentration of DPA-714 | HPLC (UV detector) | ≤0.01 mg/mL |
Chemical concentration of any impurity above disregard limit | HPLC (UV detector) | ≤0.01 mg/mL |
Sum of DPA-714 and all impurities above disregard limit | HPLC (UV detector) | ≤0.05 mg/mL |
Molar activity | HPLC (UV detector) | ≥100 GBq/µmol at EOS |
Chemical concentration tetraethylammonium (TEA) | TLC spot test | ≤0.26 mg/mL |
Bacterial endotoxins | Chromogenic kinetic method | ≤17.5 IU/mL |
Sterile filter integrity | Bubble point test | ≥2.8 bar |
After product decay | ||
Radionuclidic impurities with half-life longer than 2 h | Gamma ray spectrometer | No signal higher than 5 times background noise |
Residual solvents | Gas chromatography | Acetonitrile ≤0.41 mg/mL |
Ethanol (excipient) | Gas chromatography | ≤79 mg/mL |
Sterility | Direct inoculation | Sterile |