Table 2.

Results of method validation for selected parameters.

Parameter	Total thujone	Camphor	Rosmarinic acid derivatives		Flavon glycosides derivatives		Total carnosol derivatives	FC index	ORAC
			Rosmarinic acid	Total rosmarinic acid derivatives	Luteolin-7-Oglucuronide	Total flavon derivativesa
NMR range used for direct integration or for PLS models (δ ppm)	1.18–1.14 (2.13–2.11)	1.0–0.8 (2.50–2.40)	6.40–6.35 (7.15–7.11)	6–10	6–10	6.60–6.55	0–10	0–3	0–3
Linear range (mg/L)	1.0–1000	1–1000	20–1000	–g	–g	20–1000	–g	–g	–g
LODb (mg/L)	0.35 (1.0)f	0.92 (2.0)	10 (17)	–g	–g	7.4	–g	–g	–g
LOQb (mg/L)	1.3 (2.5)	2.2 (5.0)	19 (35)	–g	–g	26	–g	–g	–g
Precision intradayc (%)
Authentic sampled	9.6 (5.8)	0.8 (5.3)	5.6e (8.1)	12	6.3	11	11	6.8	3.5
Standard solution	8.3 (4.0)	7.3 (4.5)	6.8e (9.6)	–g	–g	1.8	–g	–g	–g
Precision interdayc (%)
Authentic sampled	11 (6.7)	3.2 (3.7)	8.8e (5.7)	8.2	8.1	10	11	4.9	5.7
Standard solution	7.3 (4.9)	6.5 (5.9)	7.1e (3.5)	–g	–g	1.7	–g	–g	–g
Recovery ranged (%)	91 (95)	98 (94)	108e (105)	108	94	90	89	102	105

Notes:

^aMeasured as luteolin-7-O-glucoside;

^bLimit of detection (LOD) and quantitation (LOQ) were determined by establishing a separate calibration curve near LODs. The limits were calculated from the residual standard deviation of the regression line;24

^cPrecisions are expressed as relative standard deviation (RSD) (%), intraday (n = 5), interday (n = 10);

^dRecovery ranges and precision for authentic samples (except total thujone and rosmarinic acid) were calculated with PLS regression models;

^eCalculated with 2D J-resolved NMR by direct integration;

^fValues for ethanol solutions are shown in brackets;

^gValue not evaluated as the parameters can only be indirectly quantified using chemometric PLS models and no pure standard was available.