Table 3 Validation summary of developed spectrofluorimetric method as per ICH guidelines
Validation as per ICH Q2 (R1) guideline for assay of PGB in pharmaceutical dosage forms | Validation as per ICH M10 guideline for analysis of spiked human plasma samples of PGB | ||
|---|---|---|---|
Validation parameter | Results | Validation parameters | Results |
Linearity range | 10 to 250 ng/mL | Linearity range | 10 to 250 ng/mL |
Regression line equation | Y = 1.7606x + 85.838 | Regression line equation | Y = 0.4468x + 154.41 |
Correlation coefficient | 0.9955 | Correlation coefficient | 0.9976 |
Repeatability of sample measurement | 0.88% (RSD) | Stability study (at 4 °C , 25 °C and −20 °C for 24 h) | 6.77–8.65% (RSD) |
Repeatability of sample preparation | 0.98% (RSD) | Carryover effect and matrix effect | 5.87–8.23% (RSD) |
Intra-day precision | 0.95–1.45% (RSD) | Intra-day precision | 6.33 – 7.45% (RSD) |
Inter-day precision | 1.23–1.98% (RSD) | Inter-day precision | 7.99–8.78% (RSD) |
%recovery | 98–102% | %recovery | 85–90% |
Limit of detection (LOQ) | 5.0 ng/mL | Lowest limit of detection (LLOD) | 5.0 ng/mL |
Limit of quantitation | 10.0 ng/mL | Lowest limit of quantitation (LLOQ) | 10.0 ng/mL |
Robustness | 1.77–1.99% (RSD) | Robustness | 8.77–9.32% (RSD) |
Specificity | specific | Specificity | Specific |