Multiscreening LC-MS/MS Designed for Ten Pesticide and Six Antimicrobial Residues in Eggs

Table 1

Evaluated compounds and results to validate multiresidue method of pesticides and antimicrobials.

Injection concentration	MRL^a [10]	MRL^b [15]	MQL^c; (μg L^−1)	R/CcA^d; (%)	R/CpA^e; (%)	RA^f; (μg L^−1) ± SD	CI^g	Lower and upper limit; (μg L^−1)
Pesticides
Ampa
5 μg L^−1	—	—	6.25	99.40	94.08		0.09	4.88–5.06
50 μg L^−1				87.40		43.70 ± 4.09	4.00	39.70–47.70
100 μg L^−1				95.43		95.43 ± 4.41	4.32	91.12–99.75
Epoxiconazole
5 μg L^−1	—	—	0,78	91,00	77,58	4.55 ± 0.57	0.56	3.99–5.10
50 μg L^−1				64,86		32.43 ± 2.03	1.99	30.44–34.42
100 μg L^−1				76,87		76.87 ± 20.36	19.95	56.92–96.81
Fipronil
5 μg L^−1	—	0.01–0.02 mg kg^−1	1.56	69.00	60.00	3.45 ± 0.05	0.05	3.41–3.50
50 μg L^−1				55.60		27.80 ± 5.87	5.75	22.05–33.55
100 μg L^−1				55.40		55.40 ± 10.43	10.22	45.18–65.62
Metolachlor
5 μg L^−1	—	—	0.78	69.20	56.17	3.46 ± 0.60	0.59	2.87–4.05
50 μg L^−1				55.20		27.60 ± 6.99	6.85	20.75–34.45
100 μg L^−1				44.10		44.10 ± 6.79	6.65	37.45–50.75
Malathion
5 μg L^−1	—	0.05 mg kg^−1	0.78	64.8	48.05	3.24 ± 1.09	1.07	2.17–4.31
50 μg L^−1				43.26		21.63 ± 4.88	4.78	16.85–26.42
100 μg L^−1				36.10		36.10 ± 7.20	7.05	29.05–43.15
Flutriafol
5 μg L^−1	—	0.40 mg kg^−1	0.78	38.00	32.25	1.90 ± 0.78	0.76	1.14–2.66
50 μg L^−1				22.94		11.47 ± 3.14	3.08	8.39–14.55
100 μg L^−1				35.80		35.80 ± 10.34	10.13	25.67–45.93
Pyraclostrobin
5 μg L^−1	—	0.02–0.05 mg kg^−1	0.78	13.60	25.43	0.68 ± 1.09	1.07	0.00–1.75
50 μg L^−1				36.74		18.37 ± 5.47	5.36	13.01–23.72
100 μg L^−1				25.95		29.25 ± 4.26	4.18	21.77–30.13
Carbendazim
5 μg L^−1	—	0.05–0.10 mg kg^−1	0.78	22.40	24.17	1.12 ± 0.05	0.05	1.07–1.17
50 μg L^−1				25.20		12.60 ± 0.27	0.26	12.34–12.86
100 μg L^−1				24.90		24.70 ± 0.75	0.74	24.16–25.34
Glyphosate
5 μg L^−1	—	0.05–150.00 mg kg^−1	0.78	17.60	19.23	0.88 ± 0.27	0.27	0.61–1.45
50 μg L^−1				20.08		10.04 ± 2.80	2.74	7.29–12.78
100 μg L^−1				20.00		20.00 ± 3.54	3.47	16.53–23.47
Carbaryl
5 μg L^−1	—	15.00–250.00 mg kg^−1	0.78	10.00	9.24	0.50 ± 0.68	0.66	0.00–1.16
50 μg L^−1				5.62		2.82 ± 1.15	1.13	1.70–3.95
100 μg L^−1				12.10		12.10 ± 4.60	4.51	7.59–16.61
Antimicrobials
Enrofloxacin
5 μg L^−1	10.00 μg L^−1	Not recommended for use in laying hens [16].	1.56	100.00	95.70	5.00 ± 0.57	0.56	4.44–5.56
50 μg L^−1				94.00		47.80 ± 8.37	8.21	39.59–56.01
100 μg L^−1				93.10		93.10 ± 13.52	13.24	82.86–109.34
Sulfamethazine
5 μg L^−1	10.00 μg L^−1	Not recommended for use in laying hens [17].	0.78	95.00	92.50	4.75 ± 0.86	0.84	3.92–5.59
50 μg L^−1				92.20		46.10 ± 3.59	3.51	42.59–49.61
100 μg L^−1				90.30		90.30 ± 2.14	2.09	88.21–92.39
Injection concentration	MRL^a [10]	MRL^b [17]	MQL^c; (μg L^−1)	R/CcA^d; (%)	R/CpA^e; (%)	RA^f; (μg L^−1) ± SD	CI^g	Lower and upper limit; (μg L^−1)
Antimicrobials
Sulfadimethoxine
5 μg L^−1	10.00 μg L^−1	—	1.56	79.80	79.73	3.99 ± 0.15	0.15	3.84–4.14
50 μg L^−1				83.40		41.70 ± 8.25	8.09	33.61–49.79
100 μg L^−1				75.98		75.98 ± 5.55	5.44	70.54–81.41
Sulfadiazine
5 μg L^−1	10.00 μg L^−1	—	1.56	66.76	72.15	3.38 ± 1.63	1.60	1.78–5.06
50 μg L^−1				69.94		34.96 ± 4.15	4.07	30.90–47.70
100 μg L^−1				79.75		79.75 ± 10.46	10.25	69.50–90.00
Chloramphenicol
5 μg L^−1	0.30 μg L^−1	There is no safe level of residues or its metabolites in food.	3.13	71.74	66.82	3.59 ± 2.01	1.95	1.07–4.97
50 μg L^−1				64.93		32.47 ± 2.31	2.27	30.20–34.73
100 μg L^−1				63.80		63.80 ± 6.28	6.15	57.65–69.95
Sulfathiazole
5 μg L^−1	10.00 μg L^−1	—	1.56	41.80	46.24	2.09 ± 0.53	0.52	1.57–2.61
50 μg L^−1				49.00		24.33 ± 5.07	4.97	19.36–29.31
100 μg L^−1				47.93		47.93 ± 11.87	11.63	36.30–59.57

MRL: maximum residue limits; ^cMQL: maximum quantification limits; ^dR/CcA: recovery/concentration averaged; ^eR/CpA: recovery/compound average; ^fRA: recovery average; ^gCI: confidence interval.