Journal of Analytical Methods in Chemistry / 2016 / Article / Tab 2 / Research Article
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 (µ g/kg) (µ g/kg) (µ g/kg) (µ g/kg) 10 (µ g/kg) 10 (µ g/kg) 25 (µ g/kg) 25 (µ g/kg) 50 (µ g/kg) 50 (µ g/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