Table 1 Validation parameters, acceptance criteria and results for HPLC method A and B
Criteria | Validation parameter | Method | No of repetitions | Aceptance Criteria | Found Method A | Found Method B |
|---|---|---|---|---|---|---|
Identity | Accuracy | Retention time [177Lu]Lu-PSMA I&T | 6 | sd (%) < 1% | 0.57% | 0.82% |
Identity | Specificity | Retention time [177Lu]Lu-PSMA I&T vs natLu-PSMA I&T | 6 | deviation < 0.5 min | 0.35 min | 0.14 min |
Radiochemical purity | (Accuracy, Precision) | Recovery calculation | 6 | Recovery 90–110% | 98.7–101.7% | 98.9–102.5% |
Radiochemical purity | Specificity | Resolution PSMA I&T vs natLu-PSMA I&T | 6 | Resolution > 3 | 6.7–7.8 | 3.7 |
Radiochemical purity | Robustness | Variation in pH, temperature, flow rate and ACN content | 1 per condition, n = 9 | Resolution [177Lu]Lu PSMA I&T and main impurity > 5 | 12.0–15.4 | 12.1–16.7 |
Radiochemical purity | Linearity | Dilution series [177Lu]Lu-DTPA, determine the correlation coefficient | 2 per dilution | R > 0.99 | 0.999 | 0.999 |
Radiochemical purity | Range | Dilution series [177Lu]Lu-DTPA, determine the concentrations between LOQ und maximum activity | 2 per dilution | 0.3–300 MBq/mL | 0.3–600 MBq/mL | 0.3–600 MBq/mL |
Radiochemical purity | LOQ | Dilution series [177Lu]Lu-DTPA, determine the concentration where peak heigth exceeds 10 × background | 2 per dilution | < 0.1% of the initial concentration of the test-solution (300 MBq/mL) | 0.05% | 0.05% |
Limit test for PSMA I&T and related substances | Linearity | Dilution series PSMA I&T | 4 per dilution | R > 0.99 | 0.999 | 0.999 |
Limit test for PSMA I&T and related substances | LOQ | Dilution series PSMA I&T, determine the concentration where peak heigth exceeds 10 × background | 4 per dilution | < 10 µg/mL | 1 µg/mL | 1 µg/mL |