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Liquid chromatography–mass spectrometry analysis of carvacrol in chicken tissues


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Fig. 1

Chromatograms obtained during validation. cps – counts per second; A and B – blank muscle sample; C and D – blank muscle sample containing carvacrol at the limit of quantification; E – internal standard
Chromatograms obtained during validation. cps – counts per second; A and B – blank muscle sample; C and D – blank muscle sample containing carvacrol at the limit of quantification; E – internal standard

Fig. 2

The proposed carvacrol fragmentation path
The proposed carvacrol fragmentation path

Fig. 3

Mass spectra of carvacrol at different collision energies. A – collision energy − 30 V; B – collision energy − 45 V; C – collision energy − 15 V
Mass spectra of carvacrol at different collision energies. A – collision energy − 30 V; B – collision energy − 45 V; C – collision energy − 15 V

Fig. 4

Chromatograms obtained during optimisation. A – Muscle sample containing carvacrol at a 10 μg g−1 concentration in negative-ion electrospray ionisation mode; B – Muscle sample containing carvacrol at a 10 μg g−1 concentration in negative-ion atmospheric pressure chemical ionisation mode
Chromatograms obtained during optimisation. A – Muscle sample containing carvacrol at a 10 μg g−1 concentration in negative-ion electrospray ionisation mode; B – Muscle sample containing carvacrol at a 10 μg g−1 concentration in negative-ion atmospheric pressure chemical ionisation mode

Fig. 5

Comparison of suitability of different extraction solvents for carvacrol
Comparison of suitability of different extraction solvents for carvacrol

Parameters obtained for the calibration curves during validation

Concentration (μg g−1) Repeatability (RSDr,%) (n = 6) Within-lab reproducibility (RSDwR,%) (n = 18) Expanded uncertainty (μg g−1) Apparent recovery (%)
Lung
0.2 3.8 ± 4.6 5.6 ± 4.4 - 103.9 ± 4.3
1.0 3.7 ± 3.6 4.8 ± 4.1 1.0 ± 0.27 107.7 ± 2.4
5.0 2.8 ± 2.9 3.2 ± 3.6 - 101.1 ± 2.5
20.0 3.2 ± 3.4 4.7 ± 3.6 - 104.9 ± 4.3
50.0 2.9 ± 3.2 4.9 ± 3.1 - 103.1 ± 4.3
Plasma
0.2 4.1 ± 3.6 5.1 ± 4.1 - 102.6 ± 5.1
1.0 3.6 ± 3.0 4.3 ± 4.2 1.0 ± 0.23 102.7 ± 3.4
5.0 3.8 ± 2.9 3.4 ± 3.3 - 103.1 ± 2.7
20.0 3.2 ± 3.7 4.0 ± 3.6 - 102.6 ± 5.1
50.0 4.1 ± 2.9 4.7 ± 3.2 - 103.6 ± 2.3
Liver
0.2 5.8 ± 4.3 6.3 ± 4.6 - 106.2 ± 7.8
1.0 4.9 ± 3.7 5.2 ± 4.3 1.0 ± 0.34 104.7 ± 4.1
5.0 3.8 ± 3.9 3.8 ± 3.7 - 104.1 ± 4.3
20.0 4.2 ± 3.0 4.7 ± 4.3 - 106.2 ± 3.8
50.0 3.7 ± 3.6 4.2 ± 3.1 - 103.2 ± 4.3
Muscle
0.2 3.8 ± 4.5 4.6 ± 4.0 - 98.9 ± 3.0
1.0 3.6 ± 3.3 4.1 ± 3.7 1.0 ± 0.26 103.2 ± 3.4
5.0 2.8 ± 3.8 3.7 ± 3.2 - 105.1 ± 3.1
20.0 3.2 ± 3.4 4.0 ± 3.2 - 99.9 ± 3.9
50.0 3.7 ± 2.9 4.1 ± 3.6 - 103.6 ± 3.5

Parameters for the multiple reaction monitoring of carvacrol

Compound Precursor ion (m/z) Product ion (m/z) DP (V) EP (V) CE (V) CXP (V)
Carvacrol 149.0 134.0 −55 −10 −22 −9
133.0 −55 −10 −38 −17
Fipronil-13C4 (IS) 438.8 333.8 −130 −10 −22 −37

Validation report for carvacrol

Matrix LOD (μg g−1) LOQ (μg g−1) Matrix effect (%) Working range (μg g−1) Determination coefficient Calibration curve
Lung 0.06 0.2 4.5 ± 1.9% 0.2–50.0 0.985 y = 0.025x + 0.04
Plasma 0.06 0.2 4.3 ± 2.7% 0.2–50.0 0.982 y = 0.065x + 0.03
Liver 0.06 0.2 6.4 ± 3.6% 0.2–50.0 0.980 y = 0.355x + 0.01
Muscle 0.06 0.2 3.3 ± 2.4% 0.2–50.0 0.991 y = 0.048x + 0.03
eISSN:
2450-8608
Sprache:
Englisch
Zeitrahmen der Veröffentlichung:
4 Hefte pro Jahr
Fachgebiete der Zeitschrift:
Biologie, Molekularbiologie, Mikrobiologie und Virologie, andere, Medizin, Veterinärmedizin