. 2022 Jun 8;70(24):7594–7606. doi: 10.1021/acs.jafc.2c01664

Table 2. Validation Parameters of the SLE–MSPE-HPLC–MS/MS Method for the Quantification of Six OAs in Bakery Products^a.

						accuracy^f		precision^f
analytes	linear range (μg/mL)	matrix-matched calibration (R²)^b	ME^c	MDL^d (μg/kg)	MQL^e (μg/kg)	recovery (% ± SD)	mean recovery (% ± SD)	intra-day precision (RSD %)	inter-day precision (RSD %)
Method Validation with Breadsticks Samples
morphine	0.01–1	y = 3.2 × 10⁶x + 1.2 × 10⁵ (0.999)	–11	6	20	71 ± 9^L	77 ± 6	17^L	20^L
						83 ± 3^H		4^H	9^H
codeine	0.01–1	y = 4.1 × 10⁶x + 7.0 × 10⁴ (1.000)	–7	13	42	75 ± 8^L	80 ± 6	13^L	18^L
						84 ± 3^H		4^H	5^H
thebaine	0.001–1	y = 2.7 × 10⁷x + 4.8 × 10⁵ (1.000)	–36	1.6	5	88 ± 10^L	83 ± 7	15^L	19^L
						77 ± 3^H		4^H	7^H
papaverine	0.001–1	y = 4.6 × 10⁷x + 1.1 × 10⁶ (0.999)	–22	3	8	66 ± 11^L	70 ± 9	19^L	19^L
						73 ± 7^H		10^H	12^H
noscapine	0.001–1	y = 7.2 × 10⁷x + 1.2 × 10⁶ (1.000)	–11	1.3	5	79 ± 9^L	81 ± 6	14^L	17^L
						83 ± 2^H		2^H	5^H
oripavine	0.01–1	y = 4.1 × 10⁶x + 4.7 × 10⁴ (0.999)	–25	13	42	85 ± 9^L	84 ± 6	14^L	17^L
						82 ± 3^H		3^H	5^H
Method Validation with Sliced Bread
morphine	0.001–1	y = 4.7 × 10⁶x + 9.5 × 10³ (1.000)	20	2	7	89 ± 9^L	90 ± 9	10^L	18^L
						90 ± 9^H		9^H	11^H
codeine	0.001–1	y = 5.2 × 10⁶x + 2.7 × 10⁵ (1.000)	17	2	7	66 ± 11^L	93 ± 9	20^L	20^L
						120 ± 7^H		6^H	7^H
thebaine	0.001–1	y = 3.9 × 10⁷x + 3.5 × 10⁷ (1.000)	–2	0.3	1	78 ± 10^L	91 ± 10	17^L	20^L
						104 ± 9^H		9^H	11^H
papaverine	0.001–1	y = 6.4 × 10⁷x + 5.3 × 10⁵ (1.000)	15	0.5	1.5	95 ± 14^L	99 ± 11	15^L	19^L
						103 ± 8^H		8^H	9^H
noscapine	0.001–1	y = 8.8 × 10⁷x + 1.6 × 10⁶ (1.000)	12	0.3	1	106 ± 4^L	110 ± 7	4^L	13^L
						114 ± 9^H		8^H	12^H
oripavine	0.01–1	y = 5.6 × 10⁶x + 5.3 × 10⁴ (1.000)	3	12	40	110 ± 10^L	105 ± 9	9^L	10^L
						100 ± 8^H		8^H	9^H

Linear range expressed in μg/kg is 80–8000 in the case of morphine, codeine, and oripavine in breadsticks and in oripavine in sliced bread and 8–8000 in all other cases.

The calibration line is in the units: μg/mL.

ME: matrix effect (dividing the purified matrix slope by the solvent slope).

MDL: method detection limit.

MQL: method quantification limit.

Accuracy and precision were obtained by spiking samples at two known concentration levels: low (L, 0.25 mg/kg) and high (H, 5 mg/kg).

Table 2. Validation Parameters of the SLE–MSPE-HPLC–MS/MS Method for the Quantification of Six OAs in Bakery Productsa.

Table 2. Validation Parameters of the SLE–MSPE-HPLC–MS/MS Method for the Quantification of Six OAs in Bakery Products^a.