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. 2021 Jul 8;10(7):1587. doi: 10.3390/foods10071587

Table 2.

Validation parameters of the SLE-MSPE-UHPLC-QqQ-MS/MS method for the determination of six opium alkaloids in poppy seeds samples.

Analytes Linear Range (µg/L) Matrix-Matched Calibration (R2) Cm ME MDLn (µg/kg) MQL (µg/kg) Accuracy Precision
Recovery (% ± SD) Mean Recovery (% ± SD) Intra-Day Precision (RSD %) Inter-Day Precision (RSD %)
Morphine 0.01–5000 y = 3269x + 32,452 (0.999) 92 64 0.07 0.24 50 ± 1 a 46 ± 2 4 a 11 a
42 ± 2 b 2 b 5 b
Codeine 0.01–5000 y = 2554x + 29,642 (0.999) 96 86 0.07 0.24 64 ± 2 a 68 ± 4 3 a 8 a
71 ± 6 b 2 b 4 b
Thebaine 0.1–5000 y = 10,093x + 485,953 (0.999) 96 109 0.72 2.40 72 ± 3 a 74 ± 4 5 a 7 a
76 ± 4 b 0 b 4 b
Papaverine 0.01–5000 y = 33,441x + 2,814,320 (0.999) 92 80 0.07 0.24 116 ± 5 a 109 ± 3 5 a 9 a
101 ± 1 b 2 b 7 b
Noscapine 0.01–5000 y = 42,914x + 1,631,091 (0.999) 94 65 0.07 0.24 109 ± 1 a 103 ± 1 4 a 10 a
97 ± 1 b 3 b 8 b
Oripavine 10–5000 y = 1080x − 31,137 (0.999) 94 31 72.07 240 51 ± 3 a 52 ± 3 3 a 5 a
53 ± 3 b 3 b 5 b

Cm: linearity coefficient calculated by (1-(SD/average slope)) × 100, where SD is the standard deviation of the calibration slopes obtained on different days; ME: matrix effect calculated by dividing the purified matrix slope by the solvent slope. MDL: method detection limit. MQL: method quantification limit estimated as 3 and 10 times the signal/noise ratio, respectively. Accuracy (mean recovery obtained from six samples, n = 6) and precision were obtained by spiking samples at two known concentration levels: a low spiked level (0.1 mg/kg) and b high spiked level (1 mg/kg). Intra-day precision: six consecutive injections (n = 6) on the same day; Inter-day precision: three replicate samples injected in triplicate throughout three different days (n = 9).