Table 5 Precision assay results of four N-nitrosamines in sartan substances.
Matrix | Compound | Spiked level (ppm) | Intraday (n = 6) | Interday (n = 18) | ||||||
|---|---|---|---|---|---|---|---|---|---|---|
Day 1 | Day 2 | Day 3 | Average recovery (%) | RSD (%) | ||||||
Average recovery (%) | RSD (%) | Average recovery (%) | RSD (%) | Average recovery (%) | RSD (%) | |||||
Candesartan cilexetil | NDMA | 3.0 | 101.06 | 3.75 | 102.37 | 2.57 | 99.40 | 3.98 | 100.94 | 3.49 |
NDEA | 0.80 | 109.56 | 4.15 | 107.83 | 3.62 | 106.31 | 5.98 | 107.90 | 4.57 | |
NDIPA | 3.0 | 97.49 | 5.50 | 95.90 | 6.38 | 93.88 | 4.74 | 95.76 | 5.49 | |
NDBA | 3.0 | 91.69 | 2.08 | 97.64 | 3.80 | 92.11 | 5.09 | 93.82 | 4.69 | |
Olmesartan medoxomi | NDMA | 2.4 | 79.76 | 4.69 | 89.26 | 4.84 | 96.31 | 4.91 | 88.45 | 9.15 |
NDEA | 0.64 | 75.07 | 1.45 | 84.66 | 3.57 | 81.84 | 6.21 | 80.52 | 6.55 | |
NDIPA | 2.4 | 91.83 | 4.32 | 83.23 | 3.57 | 82.68 | 4.28 | 86.39 | 6.05 | |
NDBA | 2.4 | 83.41 | 6.05 | 85.34 | 4.14 | 94.63 | 5.00 | 87.79 | 7.04 | |
Irbesartan | NDMA | 0.3 | 106.18 | 3.17 | 104.67 | 2.15 | 104.60 | 3.43 | 105.15 | 2.88 |
NDEA | 0.08 | 95.66 | 3.64 | 98.21 | 3.65 | 91.78 | 3.16 | 95.22 | 4.36 | |
NDIPA | 0.3 | 92.46 | 3.36 | 91.35 | 4.27 | 92.62 | 4.63 | 92.14 | 3.92 | |
NDBA | 0.3 | 114.14 | 3.85 | 109.58 | 3.45 | 116.44 | 3.99 | 113.39 | 4.40 | |
Valsartan | NDMA | 0.3 | 101.45 | 3.34 | 101.88 | 3.64 | 102.95 | 3.26 | 102.09 | 3.27 |
NDEA | 0.08 | 108.92 | 5.35 | 106.37 | 5.70 | 102.92 | 4.83 | 106.07 | 5.54 | |
NDIPA | 0.3 | 92.43 | 3.33 | 94.97 | 5.09 | 96.30 | 4.83 | 96.78 | 6.37 | |
NDBA | 0.3 | 108.74 | 4.06 | 113.88 | 4.65 | 106.21 | 3.17 | 109.61 | 4.84 | |