Analysis of Veterinary Drug and Pesticide Residues Using the Ethyl Acetate Multiclass/Multiresidue Method in Milk by Liquid Chromatography-Tandem Mass Spectrometry

Table 2

Validation results of the developed method.

Compounds		LOQ	MRL	CCα	CCβ	% recovery	% RSD	% recovery	% RSD	% recovery	% RSD	% RSDr	Relative uncertainty %	Matrix effect
		(µg/kg)	(µg/kg)	(µg/kg)	(µg/kg)	10 (µg/kg)	10 (µg/kg)	25 (µg/kg)	25 (µg/kg)	50 (µg/kg)	50 (µg/kg)
2,4-D (negative)	0.997	11	10	21	33	112	8	90	6	108	5	13	32	0.81
2,4,5-T	0.998	9	10	18	26	85	18	102	17	93	9	11	23	0.92
2,4-Dimethylaniline	0.998	8	10	18	26	79	11	110	8	97	8	11	35	0.99
Acetamiprid	0.997	10	10	18	26	97	9	102	8	96	7	11	33	0.92
Acrinathrin	0.998	11	10	18	26	106	10	88	8	104	7	11	35	0.81
Alachlor	0.997	11	10	20	30	108	11	86	4	92	3	13	28	0.81
Amitraz	0.997	9	10	20	30	86	8	76	4	76	3	14	28	0.81
Atrazine	0.997	11	10	17	23	109	6	94	5	91	3	9	30	0.85
Azoxystrobin	0.998	11	10	21	33	114	9	102	5	110	4	14	30	0.92
Bentazon	0.998	12	10	17	23	118	5	94	4	94	4	8	28	0.85
Bifenazate	0.998	11	10	20	30	109	10	102	7	111	6	11	33	0.92
Bitertanol	0.998	11	10	17	23	112	5	98	3	97	3	8	26	0.88
Boscalid	0.998	12	10	15	20	115	6	110	6	101	5	7	30	0.99
Bromacil	0.998	9	10	20	30	91	16	108	14	91	11	13	42	0.97
Bromuconazole	0.997	11	10	20	30	109	9	100	8	95	6	14	30	0.90
Bromoxynil	0.997	10	10	17	23	99	14	106	9	99	6	9	33	0.96
Bupirimate	0.997	12	10	20	30	116	5	100	5	104	3	12	26	0.90
Buprofezin	0.997	9	10	17	23	90	16	90	12	88	8	10	26	0.81
Butocarboxim sulfoxide	0.997	11	10	17	23	107	9	118	8	102	7	7	33	1.06
Cadusafos	0.997	11	10	15	20	110	11	94	8	95	5	6	30	0.85
Carbaryl	0.997	11	10	17	23	105	10	94	5	89	4	9	28	0.85
Carbendazim	0.997	12	10	20	30	118	5	122	5	113	4	11	30	1.10
Carbofuran	0.998	12	10	17	23	116	4	90	4	92	3	8	26	0.81
Carbosulfan	0.997	9	10	21	33	91	10	106	6	93	6	15	32	0.96
Carboxin	0.998	11	10	18	26	113	6	90	4	89	5	12	28	0.81
Clofentezine	0.998	9	10	17	23	88	13	98	10	93	8	10	26	0.88
Chloridazon	0.998	10	10	18	26	102	11	114	9	97	7	11	30	1.03
Chlorfenvinphos	0.998	11	10	18	26	112	8	96	5	100	3	10	30	0.86
Chlorfluazuron	0.998	11	10	21	33	107	10	114	5	108	6	14	30	1.03
Chloroxuron	0.997	11	10	18	26	108	13	102	5	104	5	10	36	0.92
Chlorpyrifos	0.997	11	10	17	23	108	9	102	6	107	6	7	32	0.92
Chlorsulfuron	0.997	10	10	21	33	96	10	92	5	88	5	15	30	0.83
Chlorthiamid	0.997	9	10	21	33	92	17	104	13	114	9	13	32	0.94
Cinidon-ethyl	0.997	11	10	17	23	105	7	100	6	110	5	8	32	0.90
Cyazofamid	0.997	11	10	18	26	112	7	94	7	93	4	10	28	0.85
Cyclanilide	0.997	12	10	21	33	115	5	104	5	113	5	13	30	0.94
Cycloate	0.998	11	10	17	23	106	12	96	11	88	5	9	28	0.86
Cymoxanil	0.998	11	10	17	23	109	7	112	6	103	6	8	32	1.01
Cyproconazole	0.998	10	10	18	26	96	10	92	6	98	4	12	28	0.83
Cyprodinil	0.998	9	10	20	30	91	16	98	9	110	9	11	30	0.88
Demeton-S-methyl	0.998	10	10	20	30	96	16	98	11	101	4	11	28	0.88
Demeton-S-methylsulfoxide	0.998	10	10	13	17	100	8	101	7	99	6	11	35	0.91
Desmedipham	0.998	10	10	13	17	99	8	98	8	87	7	14	0	0.88
Diallate	0.998	10	10	20	30	100	13	120	12	110	6	14	26	1.08
Diazinon	0.998	10	10	12	13	95	9	92	6	100	5	12	32	0.83
Dichlofluanid	0.998	10	10	17	23	103	9	104	8	100	8	12	26	0.94
Dichlorprop	0.998	9	10	18	26	88	5	88	4	95	3	8	0	0.82
Dichlorvos	0.998	9	10	15	20	93	14	118	11	109	11	16	35	1.06
Difenoconazole	0.998	9	10	15	20	92	12	100	9	94	4	11	28	0.90
Dimethenamid (sum)	0.998	11	10	17	23	112	13	98	9	87	10	10	28	0.94
Dimethoate	0.998	11	10	17	23	113	8	104	7	100	6	9	26	0.94
Dimethomorph	0.998	9	10	13	17	91	12	104	8	97	5	14	28	0.94
Dimoxystrobin	0.998	10	10	15	20	101	8	116	5	97	5	12	30	1.05
Diniconazole	0.998	10	10	13	17	97	19	96	15	87	9	10	36	0.86
Dinobuton	0.998	10	10	17	23	104	10	78	6	92	6	11	32	0.82
Dinocap (sum)	0.998	12	10	13	17	115	7	96	5	90	4	14	30	0.86
Dinoterb	0.997	12	10	18	26	115	7	100	4	98	4	9	28	0.90
Diphenylamine	0.999	12	10	13	17	115	7	108	5	90	4	14	30	0.97
Disulfoton-sulfoxide	0.997	11	10	13	17	109	10	86	6	94	5	13	30	0.82
Dithianon	0.997	11	10	13	17	106	6	108	5	102	3	6	26	0.97
Diuron	0.999	11	10	20	30	109	9	94	7	101	3	10	26	0.85
Epoxiconazole	0.997	11	10	12	13	105	8	98	4	93	4	11	28	0.88
EPTC	0.997	11	10	18	26	113	7	112	4	96	4	10	28	1.01
Ethiofencarb	0.997	12	10	18	26	115	7	96	5	96	3	9	26	0.86
Ethion	0.998	10	10	15	20	102	10	100	8	98	8	12	22	0.90
Ethirimol	0.998	10	10	15	20	98	15	96	9	111	8	13	33	0.86
Ethofumesate	0.998	11	10	17	23	105	11	96	10	100	7	13	28	0.86
Etoxazole	0.998	11	10	17	23	114	8	94	5	101	4	11	28	0.85
Ethoxyquin	0.998	10	10	13	17	100	13	96	11	98	4	11	30	0.86
Famoxadone	0.998	11	10	15	20	112	12	114	5	117	5	12	32	1.03
Fenamidone	0.998	11	10	13	17	108	9	84	8	91	6	10	26	0.82
Fenamiphos	0.998	11	10	17	23	107	5	106	4	109	3	5	32	0.96
Fenarimol	0.998	10	10	13	17	101	11	99	9	95	8	11	23	0.89
Fenazaquin	0.997	11	10	18	26	113	8	128	7	113	8	10	28	1.15
Fenbuconazole	0.997	9	10	13	17	86	16	94	12	97	4	8	32	0.85
Fenhexamid	0.997	11	10	18	26	114	7	80	6	84	5	13	28	0.82
Fenitrothion	0.997	10	10	17	23	99	12	98	11	94	9	11	24	0.88
Fenoxycarb	0.997	9	10	13	17	85	16	100	14	103	8	9	35	0.90
Fenpropathrin	0.997	10	10	18	26	100	12	100	10	99	9	7	25	0.90
Fenthion	0.997	10	10	23	36	95	12	112	11	108	7	12	33	1.01
Flazasulfuron	0.998	10	10	30	49	95	10	118	8	116	7	15	30	1.06
Fludioxonil	0.998	12	10	23	36	115	7	88	5	100	5	13	25	0.82
Fluazifop-P-butyl	0.998	12	10	28	46	118	8	102	6	96	5	11	32	0.92
Flufenacet	0.998	10	10	25	40	103	10	96	9	100	7	13	28	0.86
Flufenoxuron	0.998	10	10	26	43	95	8	100	8	105	4	11	32	0.90
Flurochloridone	0.998	10	10	18	26	100	10	102	9	112	6	7	28	0.92
Flurtamone	0.998	10	10	20	30	103	6	90	4	89	4	10	32	0.81
Flusilazole	0.998	10	10	23	36	104	8	92	6	99	6	11	32	0.83
Flutolanil	0.998	12	10	18	26	115	6	114	7	99	7	10	26	1.03
Foramsulfuron	0.998	11	10	25	40	105	4	86	3	99	4	14	26	0.82
Fosthiazate	0.997	8	10	20	30	82	13	94	5	94	3	13	30	0.85
Furathiocarb	0.997	12	10	21	33	115	5	96	5	90	5	12	33	0.86
Heptenophos	0.997	10	10	31	53	99	15	94	12	90	7	11	28	0.85
Hexythiazox	0.997	10	10	25	40	103	6	100	4	98	5	9	32	0.90
Imazalil	0.997	10	10	28	46	95	12	100	11	88	10	9	28	0.90
Imazamox	0.997	8	10	18	26	84	11	100	9	92	6	12	26	0.90
Imazaquin	0.997	11	10	31	53	112	9	90	5	86	3	12	0	0.81
Imazosulfuron	0.997	10	10	25	40	98	12	95	11	96	8	11	36	0.86
Imidacloprid	0.999	9	10	30	49	87	12	102	9	109	6	15	26	0.92
Indoxacarb	0.999	10	10	23	36	99	15	100	6	93	8	16	30	0.90
Ioxynil	0.999	10	10	20	30	99	4	84	4	81	5	8	30	0.81
Iprovalicarb	0.999	10	10	20	30	97	12	110	8	104	7	15	32	0.99
Isazofos	0.999	12	10	21	33	115	7	94	5	89	11	13	26	0.85
Isoproturon	0.999	12	10	20	30	115	8	90	6	97	6	11	38	0.81
Isoxaben	0.997	11	10	26	43	112	5	110	3	96	5	8	30	0.99
Lufenuron	0.997	10	10	26	43	99	4	98	4	94	4	13	30	0.88
Malathion	0.999	12	10	23	36	115	7	104	5	89	6	13	33	0.94
MCPA	0.997	9	10	25	40	93	9	102	5	103	7	11	28	0.92
Mecarbam	0.998	11	10	31	53	105	16	106	14	94	7	11	30	0.96
MCPP	0.998	10	10	28	46	103	12	84	9	97	9	12	41	0.82
Metalaxyl-M	0.998	10	10	23	36	97	7	122	4	101	5	16	26	1.10
Mepanipyrim	0.997	10	10	31	53	102	16	92	13	107	11	16	33	0.83
Mesosulfuron-methyl	0.997	8	10	28	46	82	15	104	5	93	6	12	35	0.94
Metazachlor	0.997	11	10	23	36	113	5	100	5	93	6	12	16	0.90
S-Metolachlor	0.999	9	10	18	26	93	8	92	7	97	7	11	27	0.83
Metosulam	0.999	11	10	30	49	110	9	94	8	88	8	14	32	0.85
Metribuzin	0.999	11	10	21	33	105	11	72	9	91	6	15	26	0.82
Monocrotophos	0.997	12	10	25	40	115	4	100	3	88	3	14	32	0.90
Monolinuron	0.997	10	10	28	46	104	17	92	14	90	8	13	28	0.83
Monuron	0.997	11	10	31	53	114	8	102	4	94	5	13	35	0.92
Omethoate	0.997	11	10	28	46	105	9	94	9	91	8	13	39	0.85
Oxadiargyl	0.997	11	10	23	36	105	15	110	11	90	11	14	30	0.99
Oxadiazon	0.997	10	10	30	49	96	8	112	5	112	5	6	32	1.01
Oxadixyl	0.997	11	10	21	33	109	12	90	10	88	6	8	35	0.81
Oxamyl	0.997	10	10	30	49	103	14	96	12	89	8	11	33	0.86
Oxasulfuron	0.997	11	10	33	56	108	8	86	8	87	7	12	28	0.82
Oxycarboxin	0.997	12	10	28	46	115	7	112	4	97	6	12	28	1.01
Oxyfluorfen	0.997	9	10	30	49	92	8	101	7	103	6	11	28	0.91
Penconazole	0.997	11	10	23	36	112	7	102	4	96	4	9	28	0.92
Pendimethalin	0.997	11	10	20	30	113	8	108	5	108	4	6	28	0.97
Pethoxamid	0.997	11	10	28	46	108	9	76	4	81	5	14	32	0.83
Phosalone	0.998	10	10	23	36	96	11	112	4	112	5	8	36	1.01
Phenmedipham	0.998	10	10	36	62	95	14	92	13	88	6	11	30	0.83
Phenthoate	0.997	12	10	23	36	115	7	94	5	89	6	12	28	0.85
Phosmet	0.997	10	10	21	33	100	11	94	10	92	9	13	33	0.85
Phosphamidon	0.997	10	10	21	33	99	8	108	7	95	7	10	30	0.97
Picloram	0.997	11	10	21	33	105	12	96	8	91	7	12	36	0.86
Picolinafen	0.997	10	10	25	40	100	12	114	9	104	9	12	25	1.03
Pirimicarb	0.997	12	10	23	36	119	8	94	2	97	3	10	30	0.85
Pirimiphos-methyl	0.997	12	10	23	36	115	7	108	5	94	5	12	30	0.97
Prochloraz	0.999	12	10	21	33	115	5	112	5	94	5	18	30	1.01
Profenofos	0.999	12	10	21	33	115	7	104	5	96	5	8	30	0.94
Prometryn	0.999	11	10	21	33	109	7	94	5	99	6	9	36	0.85
Propamocarb	0.998	10	10	25	40	100	13	102	10	89	9	11	30	0.92
Propanil	0.999	12	10	30	49	115	7	102	5	99	6	12	28	0.92
Propargite	0.999	10	10	26	43	102	14	112	10	113	4	8	30	1.01
Propham	0.999	10	10	21	33	102	13	100	6	96	5	10	28	0.90
Propiconazole	0.999	10	10	30	49	98	6	122	4	111	6	14	30	1.10
Propyzamide	0.999	8	10	28	46	84	10	96	9	95	5	9	33	0.86
Pymetrozine	0.997	10	10	23	36	101	10	96	8	90	7	11	28	0.86
Pyraclostrobin	0.997	12	10	21	33	115	7	130	5	119	4	15	26	1.17
Pyridaben	0.997	9	10	20	30	89	16	80	12	81	4	11	36	0.82
Pyridaphenthion	0.997	10	10	23	36	99	11	120	9	99	10	13	26	1.08
Pyridate	0.998	10	10	31	53	98	5	106	4	98	3	8	32	0.96
Pyriproxyfen	0.997	10	10	21	33	101	11	94	6	86	5	13	22	0.85
Quinalphos	0.997	10	10	23	36	101	5	76	6	90	5	14	23	0.82
Quinoxyfen	0.999	10	10	30	49	99	5	98	1	100	2	8	23	0.88
Quizalofop-P-ethyl	0.997	12	10	30	49	115	7	82	5	85	5	14	26	0.84
Rimsulfuron	0.998	9	10	26	43	88	13	104	3	100	2	14	26	0.94
Simazine	0.997	11	10	23	36	106	16	96	8	99	3	11	23	0.86
Spiroxamine	0.999	8	10	21	33	83	14	84	9	82	2	14	32	0.82
Sulfosulfuron	0.997	8	10	21	33	82	12	110	6	111	6	19	30	0.99
Tebuconazole	0.999	10	10	28	46	99	10	94	6	99	5	9	25	0.85
TEPP	0.997	9	10	23	36	90	7	107	7	105	6	11	29	0.96
Terbutryn	0.997	12	10	26	43	115	8	96	5	102	3	11	28	0.86
Terbuthylazine	0.997	10	10	20	30	104	12	118	5	116	4	6	26	1.06
Tetrachlorvinphos	0.997	11	10	21	33	113	11	78	8	90	4	14	28	0.90
Thiabendazole	0.997	12	10	21	33	118	6	98	4	96	5	13	30	0.88
Thiacloprid	0.997	11	10	18	26	106	13	84	12	89	5	8	35	0.82
Thiamethoxam	0.997	10	10	33	56	104	19	118	11	113	8	11	32	1.06
Thifensulfuron-methyl	0.997	9	10	20	30	91	16	98	8	92	9	15	30	0.88
Thiodicarb	0.997	12	10	31	53	115	7	102	5	97	6	9	35	0.92
Thiophanate-methyl	0.997	11	10	20	30	114	9	112	6	95	5	13	32	1.01
Triadimefon	0.997	10	10	28	46	104	7	106	6	98	5	8	32	0.96
Triadimenol	0.997	11	10	25	40	107	14	106	6	92	7	9	26	0.96
Triallate	0.998	11	10	23	36	106	9	114	3	111	4	12	30	1.03
Triasulfuron	0.998	11	10	20	30	111	8	76	5	91	6	14	30	0.82
Triazophos	0.998	12	10	30	49	115	7	96	5	87	5	9	30	0.86
Tribenuron-methyl	0.998	10	10	35	59	99	9	103	8	101	5	11	30	0.93
Tributylphosphate	0.997	10	10	17	23	104	14	88	12	89	5	8	35	0.81
Trichlorfon	0.998	10	10	25	40	98	10	104	3	100	2	14	27	0.94
Tridemorph	0.997	10	10	21	33	98	17	90	13	100	5	11	30	0.81
Trifloxystrobin	0.997	12	10	25	40	115	7	124	5	114	5	14	30	1.12
Triflumizole	0.997	11	10	20	30	113	14	92	5	99	5	8	28	0.83
Triticonazole	0.998	10	10	17	23	100	11	106	10	98	7	7	32	0.96
Vamidothion	0.997	9	10	21	33	93	13	118	6	102	7	16	28	1.06
Zoxamide	0.997	12	10	23	36	116	7	72	4	85	3	15	25	0.82
Ciprofloxacin	0.997	7	100	124	148	74	25	61	16	97	13	9	38	0.81
Clindamycin	0.997	11	10	12	14	110	23	106	15	109	10	12	34	0.96
Chlortetracycline	0.999	10	100	108	116	101	7	93	7	99	6	9	14	0.84
Danofloxacin	0.999	10	30	40	48	104	14	87	12	88	8	9	24	0.82
Difloxacin	0.999	9	10	11	13	87	8	100	7	96	6	10	15	0.90
Doxycycline hydrate	0.999	10	100	110	119	104	14	93	11	96	8	10	23	0.84
Flumequine	0.998	9	50	54	58	88	12	105	11	93	10	11	22	0.95
Josamycin	0.998	9	10	11	13	88	12	104	11	97	9	12	22	0.94
Lomefloxacin	0.999	10	10	12	13	99	13	89	11	99	8	10	22	0.80
Orbifloxacin	0.999	9	10	11	12	93	14	107	8	94	7	11	20	0.96
Oxolinic acid	0.999	11	10	12	15	110	12	102	10	102	6	15	20	0.92
Oxytetracycline	0.999	11	100	111	122	114	15	104	12	95	6	10	23	0.94
Rifampicin	0.997	10	10	11	13	98	9	85	8	98	5	9	15	0.81
Sarafloxacin	0.997	10	10	12	14	101	10	97	8	102	5	11	16	0.87
Sulfachloropyridazine	0.997	9	100	116	132	88	13	106	12	80	9	10	24	0.96
Sulfaquinoxaline	0.998	10	100	111	122	97	15	99	10	78	9	9	24	0.89
Sulfadiazine	0.997	8	100	108	116	85	12	98	9	98	5	10	18	0.88
Sulfamerazine	0.999	8	100	111	122	85	12	104	8	75	7	9	19	0.94
Sulfathiazole	0.999	9	100	113	126	85	11	109	10	81	10	17	21	0.98
Sulfamethazine	0.999	8	100	114	129	84	13	104	9	104	8	11	21	0.94
Sulfadoxine	0.999	9	100	114	129	88	16	95	12	95	6	10	24	0.86
Sulfapyridine	0.997	8	100	119	138	83	11	108	10	96	8	10	20	0.97
Sulfaclozine	0.998	10	100	111	122	99	10	92	8	98	5	9	16	0.83
Sulfamethoxazole	0.998	10	100	116	132	102	9	95	7	87	5	9	15	0.86
Tilmicosin	0.999	10	50	56	62	98	12	104	9	105	4	10	18	0.94
Tetracycline	0.999	10	100	119	138	100	18	84	8	96	5	9	23	0.82