Chemical assessment of mycotoxin contaminants and veterinary residues in Costa Rican animal feed

Leiva, Astrid; Méndez, Geovanna; Rodríguez, César; Molina, Andrea; Granados-Chinchilla, Fabio

doi:10.1186/s40550-019-0075-8

Food Safety and Risk

Table 1 Performance parameters and mass detector settings for the assessed analytes in order of increasing molar mass

From: Chemical assessment of mycotoxin contaminants and veterinary residues in Costa Rican animal feed

Analyte	Molar mass, g/mol	Retention time, min	Target ion, m/z	Fragmentor	Dwell time, ms	Calibration curve equation^a or response factor	^bLimit of detection, μg kg^− 1 (^cμg L^− 1)	Limit of quantification, μg kg^− 1
Mycotoxin contaminants
Patulin	154.21	24.63	154.3 [M+]	120	71	y = (4.81 × 10³ ± 2.69 × 10²)x	0.62 (10.1)	1.84
Citrinin	251.10	23.48	251.0 [M+]	120	56	y = (3.67 × 10³ ± 8.11 × 10²)x	0.34 (1.9)	1.03
Deoxynivalenol	296.30	8.69	297.1 [M + H]⁺ and 319.0 [M + Na]⁺	120	144	y = (1.61 × 10³ ± 4.11 × 10²)x	6.31 (105.2)	19.12
Aflatoxin B₁	312.28	21.11	313.0 [M + H]⁺	140	34	y = (2.62 × 10² ± 3.14 × 10¹)x	0.40 (6.7)	1.21
Nivalenol	312.32	5.14	355.1 [M + 2Na]⁺	140	143	y = (1.73 × 10² ± 2.10 × 10¹)x	6.42 (107.0)	19.45
Aflatoxin B₂	314.30	20.48	315.0 [M + H]⁺	140	34	y = (1.01 × 10² ± 3.15 × 10¹)x	0.14 (2.3)	0.42
Zearalenone	318.40	24.67	319.0 [M + H]⁺	120	71	y = (6.75 × 10² ± 3.41 × 10¹)x	0.26 (4.3)	0.79
β-zearalenol	320.38	22.16	321.0 [M + H]⁺	120	56	y = (1.43 × 10² ± 2.55 × 10¹)x	0.44 (7.3)	1.33
α-zearalenol	320.38	23.07	321.1 [M + H]⁺	120	56	y = (4.80 × 10³ ± 2.01 × 10²)x	0.63 (5.67)	1.91
Sterigmatocystin	324.30	25.43	327.1 [M + 3H]⁺	140	95	y = (7.64 × 10² ± 5.54 × 10¹)x	0.60 (10.0)	1.82
Aflatoxin G₁	328.30	20.48	328.9 [M + H]⁺	140	34	y = (5.95 × 10² ± 2.33 × 10¹)x	0.27 (4.5)	0.82
Aflatoxin M₁	328.27	19.13	329.0 [M + H]⁺	140	34	y = (4.02 × 10³ ± 3.61 × 10²)x	0.005 (0.8)	0.02
Aflatoxin G₂	330.30	19.87	331.0 [M + H]⁺	140	34	y = (1.10 × 10² ± 1.12 × 10¹)x	0.20 (3.3)	0.61
3-acetoxydeoxynivalenol	338.35	18.01	339.2 [M + H]⁺	140	71	y = (1.78 × 10² ± 6.65 × 10¹)x	0.38 (6.3)	1.15
15-acetoxydeoxynivalenol	338.35	18.26	339.1 [M + H]⁺	120	71	y = (8.77 × 10² ± 2.15 × 10¹)x	0.30 (5.0)	0.91
Fusarenon-X	354.35	15.74	355.0 [M + H]⁺	140	71	y = (1.40 × 10² ± 1.17 × 10¹)x	0.29 (4.8)	0.88
Diacetoxyscirpenol	366.41	16.84	365.0 [C₁₉H₂₅O₇]⁺˙ - H˙	140	71	y = (8.35 × 10¹ ± 4.31 × 10⁰)x	0.32 (5.3)	0.97
Ochratoxin B	369.37	22.71	370.0 [M + H]⁺	120	56	y = (1.23 × 10² ± 1.15 × 10¹)x	0.21 (3.5)	0.64
Neosolaniol	382.41	20.79	384.2 [M + 2H]⁺	140	34	y = (8.74 × 10² ± 9.14 × 10¹)x	0.61 (10.2)	1.85
Ochratoxin A	405.40	24.35	404.0 [M + H]⁺	120	71	y = (1.19 × 10² ± 5.09 × 10¹)x	0.16 (2.7)	0.48
HT-2 toxin	424.48	21.38	425.1 [M + H]⁺	140	56	y = (1.06 × 10³ ± 2.19 × 10²)x	0.32 (5.3)	0.97
T-2 toxin	466.47	22.66	484.3 [M + NH₄]⁺	140	71	y = (8.78 × 10² ± 4.54 × 10¹)x	0.96 (16.0)	2.91
Enniatin B	639.83	29.94	640.3 [M + H]⁺	120	95	y = (3.50 × 10² ± 1.07 × 10¹)x	1.16 (19.2)	3.50
Enniatin B₁	653.86	30.98	654.3 [M + H]⁺	120	95	y = (2.00 × 10³ ± 2.01 × 10²)x	0.11 (1.8)	0.34
Fumonisin B₁	721.84	18.88	723.2 [M + 2H]⁺	100	34	y = (1.19 × 10³ ± 1.27 × 10²)x	0.08 (1.3)	0.24
Fumonisin B₂	705.84	20.09	706.2 [M + H]⁺	100	34	y = (3.20 × 10² ± 3.23 × 10¹)x	0.43 (7.17)	1.30
Veterinary residues
Sulfamethazine	278.33	9.18	279.0 [M + H]⁺	120	146	2.61 × 10⁴ ± 6.91 × 10³	45.45 (50)	151.52
Spectinomycin	332.35	1.18	333.1 [M + H]⁺	140	97	7.53 × 10² ± 1.91 × 10¹	68.18 (75)	227.27
Florfenicol	358.20	13.15	339.9 [C₁₂H₁₄Cl₂NO₄S]⁺˙ - F˙	120	97	1.33 × 10² ± 2.32 × 10¹	45.45 (50)	151.52
Cloramphenicol	323.13	14.51	344.9 [M + Na]⁺	120	97	3.02 × 10² ± 9.11 × 10¹	46.36 (51)	154.55
Penicillin G	334.39	17.28	354.0 [M + Na]⁺ and 367.0 [M + 2H₂O]⁺	60	83	1.75 × 10³ ± 2.67 × 10²	97.27 (107)	324.24
Lincomycin	406.54	7.23	407.1 [M + H]⁺	120	146	4.32 × 10³ ± 1.41 × 10²	81.82 (90)	272.73
4-epianhydrotetracycline	426.42	14.77	427.0 [M + H]⁺	120	97	1.27 × 10³ ± 5.44 × 10²	100.01 (105)	303.03
Methacycline	442.42	13.68	443.0 [M + H]⁺	120	97	2.33 × 10² ± 7.83 × 10¹	57.27 (63)	190.91
Tetracycline	444.44	10.12	445.0 [M + H]⁺	120	97	2.00 × 10³ ± 4.23 × 10²	41.82 (46)	139.39
Doxycycline	444.44	14.08	446.0 [M + 2H]⁺	120	97	1.17 × 10² ± 5.67 × 10¹	83.64 (92)	278.79
4-epitetracycline	444.44	10.23	447.1 [M + 3H]⁺	140	97	3.19 × 10² ± 3.23 × 10¹	90.91 (100)	275.48
Minocycline	457.48	7.14	458.1 [M + H]⁺	120	146	1.25 × 10³ ± 1.01 × 10²	71.21 (83)	254.38
Demeclocycline	464.85	11.43	465.0 [M + H]⁺	120	97	1.12 × 10³ ± 7.34 × 10²	41.82 (46)	139.39
Oxytetracycline	460.44	9.46	461.0 [M + H]⁺	140	97	2.27 × 10² ± 6.51 × 10¹	82.73 (91)	275.76
4-epioxytetracycline	460.44	9.42	462.3 [M + 2H]⁺	120	146	2.94 × 10² ± 2.21 × 10¹	101.02 (113)	368.63
Chlortetracycline	478.88	13.10	479.0 [M + H]⁺	120	97	1.25 × 10³ ± 5.55 × 10²	92.12 (102)	301.06
4-epichlortetracycline	478.88	11.57	479.1 [M + H]⁺	120	97	6.51 × 10² ± 3.48 × 10¹	132.73 (146)	442.42
Virginimycin M₁	525.60	21.94	526.1 [M + H]⁺	120	83	4.46 × 10³ ± 2.46 × 10²	59.09 (65)	196.97
Monensin A	670.88	24.56	693.2 [M + Na]⁺	180	83	1.13 × 10⁴ ± 1.01 × 10³	40.91 (45)	136.36
Erythromycin	733.94	16.83	734.3 [M + H]⁺	140	83	1.16 × 10⁴ ± 1.76 × 10³	80.93 (89)	264.56
Narasin	765.04	25.20	787.3 [M + Na]⁺	260	83	1.26 × 10³ ± 2.26 × 10²	24.55 (27)	81.82
Virginimycin S₁	823.90	23.35	824.1 [M + H]⁺	120	83	3.47 × 10³ ± 3.44 × 10²	59.09 (65)	196.97
Tylosin	916.11	18.05	916.2 [M+]	140	83	5.37 × 10³ ± 2.88 × 10²	45.45 (48)	151.52

^aAll trend line intercepts adjusted to zero as their values are deemed negligible with respect to the slopes and areas. The equations shown are the result of an average of three curves measured independently and under reproducibility conditions
^bLimit of detection and quantification calculated as S/N ratio times 3.3 and 10, respectively. Values corroborated by extinction assays
^cSmallest concentration detected for each analyte within the calibration curve (experimental data)

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