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. 2020 Oct 19;9(10):1497. doi: 10.3390/foods9101497

Table 1.

Linearities, curves, LODs and LOQs and method validation parameters for the analysis of 116 target a.is. in tomato in LC-MS/MS.

Pesticide Linearity Linear Regression Equation R2 ± RSD% MRL LOD LOQ Apparent Recovery (%, n = 15) RSDr (5×LOQ) RSDwR (5×LOQ) U *
(g kg−1) (mg kg−1) (g kg−1) (g kg−1) LOQ 10xLOQ n = 30 n = 60
Cyromazine LOQ–411 y = 2741924x + 8425 0.9988 ± 0.07 0.60 1.37 4.11 115.3 ± 4.9 108.8 ± 1.7 11.2 12.4 29.4
Methamidophos LOQ–410 y = 4887931x + 21107 0.9989 ± 0.06 0.01 * 1.37 4.10 105.4 ± 14.3 93.1 ± 10.8 9.0 12.9 38.3
Acephate LOQ–435 y = 375881x − 144 1.0000 ± 0.10 0.01 * 1.45 4.35 96.5 ± 13.3 90.6 ± 19.4 12.0 17.1 39.8
Formetanate LOQ–413 y = 14913520x − 5868 1.0000 ± 0.01 0.30 1.38 4.13 84.5 ± 1.9 84.4 ± 9.3 8.6 16.9 33.6
Pymetrozine LOQ–473 y = 696973x + 6250 0.9959 ± 0.08 0.50 1.58 4.73 101.3 ± 6.7 98.2 ± 5.8 13.9 14.0 16.5
Omethoate LOQ–621 y = 32351x + 372 0.9987 ± 0.07 0.01 * 2.07 6.21 87.4 ± 7.5 85.1 ± 5.9 7.5 15.1 31.8
Propamocarb LOQ–417 y = 43247201x − 8829 0.9998 ± 0.18 4.00 1.39 4.17 99.6 ± 6.7 98.5 ± 2.7 13.5 12.9 14.3
Oxamyl LOQ–401 y = 5159083x − 5579 1.0000 ± 0.01 0.01 1.34 4.01 94.8 ± 11.1 80.9 ± 0.3 5.3 8.1 38.6
Methomyl LOQ–410 y = 5917725x + 7746 0.9997 ± 0.14 0.01 1.37 4.10 111.8 ± 10.4 107.2 ± 2.3 9.6 10.3 31.0
Flonicamid LOQ–394 y = 784761x + 1544 0.9998 ± 0.13 0.50 1.31 3.94 95.5 ± 9.6 91.0 ± 12.9 15.4 11.4 29.4
Thiamethoxam LOQ–524 y = 11189678x + 71281 0.9986 ± 0.08 0.20 1.75 5.24 107.8 ± 8.3 104.5 ± 2.5 7.4 9.8 22.6
Carbendazim LOQ–400 y = 5329930x + 3082 1.0000 ± 0.01 0.30 * 1.33 4.00 76.6 ± 1.7 83.7 ± 4.1 8.1 12.8 43.2
Monocrotophos LOQ–414 y = 17644763x + 44731 0.9993 ± 0.11 0.01 * 1.38 4.14 96.4 ± 11.1 79.8 ± 7.4 6.5 10.7 41.8
Chlordimeform LOQ–396 y = 853728x − 1979 0.9998 ± 0.01 - 1.32 3.96 85.6 ± 7.4 75.5 ± 0.7 14.2 11.4 43.1
Cypermethrin LOQ–518 y = 5132597x + 20901 0.9979 ± 0.12 0.50 1.73 5.18 86.6 ± 4.1 86.3 ± 7.4 12.6 11.8 29.7
Imidacloprid LOQ–321 y = 5358564x + 20834 0.9990 ± 0.20 0.50 1.07 3.21 107.4 ± 13.7 107.0 ± 1.2 4.2 6.7 32.1
Methiocarb LOQ–387 y = 31899495x + 73553 0.9994 ± 0.16 0.20 1.29 3.87 76.9 ± 1.9 80.0 ± 5.2 5.6 9.0 44.7
Dimethoate LOQ–407 y = 9144917x + 45650 0.9984 ± 0.08 0.02 1.36 4.07 105.3 ± 5.0 96.7 ± 2.7 12.3 8.4 17.7
Acetamiprid LOQ–398 y = 13742437x + 39503 0.9992 ± 0.79 0.50 1.33 3.98 98.1 ± 8.7 88.1 ± 1.8 6.1 10.7 26.7
Cymoxanil LOQ–435 y = 7081921x + 5097 0.9998 ± 0.00 0.40 1.45 4.35 99.1 ± 5.8 88.6 ± 5.8 11.4 14.9 24.1
Thiacloprid LOQ–439 y = 4714164x + 21318 0.9988 ± 0.55 0.50 1.46 4.39 111.8 ± 5.7 106.6 ± 1.2 11.2 12.8 24.4
Atrazine-desethyl LOQ–430 y = 8730484x + 17192 0.9996 ± 0.03 - 1.43 4.30 102.0 ± 5.2 93.5 ± 3.8 8.4 11.5 18.0
Aldicarb LOQ–458 y = 22774x − 3 0.9989 ± 0.04 0.02 * 1.53 4.58 99.8 ± 0.2 99.9 ± 0.2 10.0 8.1 10.6
Pirimicarb LOQ–410 y = 30848679x + 25212 0.9994 ± 0.02 0.50 1.37 4.10 109.8 ± 9.6 108.2 ± 1.8 9.5 7.8 27.7
Dichlorvos LOQ–410 y = 450147x + 175 1.0000 ± 0.01 0.01 * 1.37 4.10 87.2 ± 4.3 81.7 ± 2.0 8.7 17.1 32.6
Thiophanate-methyl LOQ–406 y = 17268518x − 53036 0.9997 ± 0.32 1.00 1.35 4.06 93.1 ± 10.0 80.2 ± 4.6 18.1 7.9 38.4
Metribuzin LOQ–427 y = 3761325x + 17279 0.9983 ± 0.74 0.10 1.42 4.27 98.9 ± 10.7 108.4 ± 2.4 5.6 12.4 26.3
Carbofuran LOQ–416 y = 27252840x + 33458 0.9996 ± 0.01 0.002 * 1.39 4.16 96.3 ± 2.9 94.9 ± 1.5 8.5 7.7 10.7
Carbaryl LOQ–410 y = 14046644x + 7098 0.9998 ± 0.22 0.01 * 1.37 4.10 110.4 ± 5.0 100.2 ± 2.1 8.4 11.5 22.9
Imazalil LOQ–431 y = 972258x + 947 0.9999 ± 0.21 0.50 1.44 4.31 78.8 ± 8.2 77.5 ± 2.2 13.0 16.7 46.0
Fosthiazate LOQ–397 y = 720338x + 1656 0.9997 ± 0.12 0.02 1.32 3.97 97.2 ± 2.1 98.7 ± 0.1 7.5 10.6 6.4
Disulfoton-Sulfoxide LOQ–471 y = 12702349x + 19964 0.9998 ± 0.32 - 1.57 4.71 110.8 ± 7.0 107.6 ± 1.2 4.6 16.4 24.7
Flutriafol LOQ–470 y = 3625x + 183 0.9986 ± 0.04 0.80 1.57 4.70 106.9 ± 8.1 104.9 ± 1.0 15.2 12.4 21.0
Metalaxyl LOQ–390 y = 4371x + 183 0.9986 ± 0.04 0.20 1.30 3.90 85.6 ± 6.9 84.3 ± 13.1 9.5 10.2 36.7
Methidathion LOQ–424 y = 396329x − 101 0.9994 ± 0.14 0.02 * 1.41 4.24 93.6 ± 11.4 92.9 ± 2.9 10.2 11.1 26.2
Azinphos-methyl LOQ–464 y = 398216x + 390 0.9998 ± 0.58 0.05 * 1.55 4.64 98.2 ± 9.9 93.6 ± 2.3 8.5 19.4 22.5
Chlorantraniliprole LOQ–399 y = 585240x + 2 0.9997 ± 0.01 0.60 1.33 3.99 92.1 ± 5.8 89.6 ± 4.5 7.4 15.7 22.2
Pyrimethanil LOQ–395 y = 1208059x − 4250 0.9991 ± 0.05 1.00 1.32 3.95 109.7 ± 5.5 105.4 ± 0.3 7.4 15.7 20.9
Azoxystrobin LOQ–431 y = 37027632 + 20546 0.9999 ± 0.31 3.00 1.44 4.31 103.4 ± 5.5 99.7 ± 4.2 6.7 19.8 14.5
Diethofencarb LOQ–385 y = 17914008x +75801 0.9990 ± 1.21 0.70 * 1.28 3.85 97.0 ± 14.2 83.9 ± 14.6 6.4 15.5 43.4
Propanil LOQ–392 y = 1172102x − 4083 0.9972 ± 0.09 0.01 * 1.31 3.92 90.9 ± 5.1 91.0 ± 5.8 12.5 13.0 22.0
Fenamidone LOQ–390 y = 19532597x + 43718 0.9995 ± 1.06 1.00 1.30 3.90 96.5 ± 9.5 103.2 ± 1.3 9.4 14.5 21.5
Diclobutrazol LOQ–391 y = 145538x + 476 0.9993 ± 0.22 - 1.30 3.91 101.5 ± 0.7 102.0 ± 0.2 8.7 10.3 3.8
Boscalid LOQ–408 y = 4252887x + 877 1.0000 ± 0.30 3.00 1.36 4.08 104.5 ± 8.6 105.9 ± 0.3 14.1 15.5 20.6
Dimethomorph LOQ–394 y = 14639124x + 39105 0.9980 ± 0.16 1.00 1.31 3.94 93.8 ± 17.4 97.9 ± 2.5 8.9 8.7 35.5
Mandipropamid LOQ–455 y = 5148550x − 20963 0.9983 ± 5.08 3.00 1.52 4.55 85.6 ± 11.9 82.1 ± 8.4 5.6 14.8 40.6
Benthiavalicarb LOQ–235 y = 4160577x + 5366 0.9994 ± 0.97 0.30 0.78 2.35 111.4 ± 5.8 106.8 ± 0.9 9.7 11.5 24.0
Molinate LOQ–621 y = 47567x − 140 0.9999 ± 0.93 0.01 * 2.07 6.21 92.2 ± 3.1 85.9 ± 4.6 8.1 15.4 24.5
Chloroxuron LOQ–425 y = 12252052x − 45885 0.9984 ± 0.19 0.01 * 1.42 4.25 105.7 ± 5.7 102.3 ± 0.4 4.5 10.5 15.7
Myclobutanil LOQ–411 y = 123049x − 122 0.9997 ± 0.07 0.30 1.37 4.11 83.1 ± 6.1 91.8 ± 0.7 13.4 13.7 32.5
Bifenazate LOQ–399 y = 1008299x + 76836 0.9961 ± 1.07 0.50 1.33 3.99 87.0 ± 14.1 90.8 ± 19.6 5.6 15.5 44.4
Cyproconazole 1 LOQ–410 y = 14106016x + 110236 0.9985 ± 4.29 0.05 1.37 4.10 109.2 ± 7.2 105.7 ± 1.1 10.8 18.6 22.6
Triadimenol LOQ–495 y = 3828694x + 27482 0.9970 ± 5.79 1.00 1.65 4.95 84.9 ± 13.3 96.4 ± 8.1 8.4 15.7 38.8
Iprovalicarb LOQ–408 y = 4408560x + 40826 0.9967 ± 0.22 0.70 1.36 4.08 90.6 ± 14.0 102.9 ± 0.4 12.4 13.5 33.7
Fenhexamid LOQ–436 y = 3699942x + 18108 0.9991 ±1.57 2.00 1.45 4.36 102.8 ± 5.9 82.3 ± 3.6 3.4 18.5 36.8
Azinphos-ethyl LOQ–391 y = 367433x + 492 0.9997 ± 0.39 0.02 * 1.30 3.91 79.1 ± 9.5 95.7 ± 0.5 7.6 15.4 43.2
Tetraconazole LOQ–516 y = 9182219x − 30061 0.9993 ± 0.09 0.10 1.72 5.16 106.8 ± 7.4 109.5 ± 0.9 12.1 15.3 22.4
Cyproconazole 2 LOQ–410 y = 5446075x − 17111 0.9994 ± 5.95 0.05 1.37 4.10 105.3 ± 7.5 102.7 ± 1.1 7.7 13.5 18.3
Mepanipyrim LOQ–407 y = 328904x − 348 0.9991 ± 2.87 1.50 1.36 4.07 96.6 ± 2.1 100.8 ± 0.6 13.3 19.1 8.5
Spirotetramat LOQ–503 y = 2820842x + 73839 0.9997 ± 0.67 2.00 1.68 5.03 85.6 ± 5.6 98.5 ± 1.7 6.5 18.3 29.9
Flufenacet LOQ–414 y = 10522988x + 50386 0.9983 ± 8.65 0.05 1.38 4.14 89.9 ± 8.6 89.9 ± 0.4 10.5 14.8 28.4
Ethoprop LOQ–377 y = 5056608x + 20031 0.9990 ± 2.42 0.02 1.26 3.77 89.5 ± 10.1 88.4 ± 1.2 8.9 10.4 29.2
Bupirimate LOQ–396 y = 7147770x + 5118 0.9998 ± 0.37 2.00 1.32 3.96 91.8 ± 4.5 81.9 ± 10.2 5.4 18.8 33.1
Cyazofamid LOQ–405 y = 54070x + 229 0.9992 ± 0.72 0.60 1.35 4.05 101.7 ± 1.0 102.7 ± 0.2 5.6 12.8 5.0
Flusilazole LOQ–457 y = 9842141x + 54831 0.9982 ± 2.81 0.01 * 1.52 4.57 106.4 ± 8.2 104.1 ± 0.2 5.8 14.9 20.7
Cyprodinil LOQ–408 y = 2997671x + 13504 0.9992 ± 0.05 1.50 1.36 4.08 93.9 ± 15.1 79.8 ± 1.9 4.6 18.7 45.0
Fenamiphos LOQ–547 y = 2610314x + 116029 0.9991 ± 0.92 0.04 1.82 5.47 103.9 ± 7.1 100.7 ± 1.2 11.2 15.6 16.5
Iprodione LOQ–455 y = 82937x + 89 0.9997 ± 0.22 5.00 1.52 4.55 94.4 ± 4.0 96.5 ± 4.2 9.9 15.8 14.0
Aclonifen LOQ–393 y = 96057x + 89 0.9997 ± 0.22 0.01 1.31 3.93 97.5 ± 1.2 96.2 ± 0.7 12.4 12.5 7.0
Penconazole LOQ–398 y = 6090424x + 15097 0.9992 ± 0.43 0.10 1.33 3.98 104.6 ± 6.2 102.4 ± 0.1 9.1 11.4 15.2
Tebuconazole LOQ–401 y = 19544180x + 77610 0.9989 ± 0.56 0.90 1.34 4.01 102.1 ± 2.1 104.4 ± 1.1 7.1 10.4 8.4
Napropamide LOQ–413 y = 6724980x + 62380 0.9964 ± 0.81 0.10 1.38 4.13 108.4 ± 6.2 104.8 ± 11.1 8.5 13.8 25.6
Benalaxyl LOQ–481 y = 23788991x + 92142 0.9982 ± 0.19 0.50 1.60 4.81 100.6 ± 4.9 108.6 ± 1.1 8.9 9.4 17.4
Spinosyn A LOQ–432 y = 1125007x − 3076 0.9997 ± 0.01 0.70 1.44 4.32 77.0 ± 4.1 76.7 ± 0.6 15.5 14.5 46.8
Zoxamide LOQ–410 y = 5772043x + 12727 0.9994 ± 0.04 0.5 1.37 4.10 92.1 ± 9.4 81.5 ± 4.8 16.5 13.2 35.7
Pyraclostrobin LOQ–418 y = 13354734x − 5243 1.0000 ± 3.84 0.30 1.39 4.18 94.5 ± 8.2 92.8 ± 3.9 5.8 15.7 21.0
Cyflufenamid LOQ–408 y = 5945864x + 38431 0.9977 ± 0.65 0.04 1.36 4.08 87.5 ± 17.6 91.1 ± 1.1 17.4 18.5 40.0
Bitertanol LOQ–406 y = 6031192x + 40609 0.9969 ± 0.80 0.01 * 1.35 4.06 105.1 ± 1.7 102.6 ± 0.9 11.2 14.6 9.8
Clofentezin LOQ–408 y = 1910622x − 533 0.9999 ± 0.95 0.30 1.36 4.08 83.2 ± 11.4 103.7 ± 3.8 8.9 8.1 42.8
Phosalone LOQ–578 y = 6702437x + 16186 0.9995 ± 0.02 0.01 * 1.93 5.78 99.6 ± 3.4 94.2 ± 3.1 3.4 12.8 12.8
Metrafenone LOQ–468 y = 9239760x + 20728 0.9999 ± 0.02 0.40 1.56 4.68 96.4 ± 1.9 101.0 ± 4.9 5.6 8.4 11.4
Difenconazole LOQ–485 y = 20779327x + 20116 0.9999 ± 0.02 2.00 1.62 4.85 97.4 ± 7.3 95.8 ± 1.8 10.0 9.4 16.3
Chlorpyrifos-methyl LOQ–414 y = 65820x − 225 0.9999 ± 0.71 0.50 1.38 4.14 91.2 ± 7.9 79.1 ± 2.3 9.1 11.4 37.5
Ametoctradin LOQ–317 y = 8626247x + 1875 0.9999 ± 0.01 2.00 1.06 3.17 96.1 ± 7.1 92.8 ± 0.4 8.4 18.7 18.2
Spinosyn D LOQ–432 y = 209477x − 615 0.9997 ± 0.41 0.70 1.44 4.32 92.9 ± 7.6 89.4 ± 4.1 12.7 5.6 23.8
Indoxacarb LOQ–450 y = 1790071x − 2915 0.9985 ± 0.01 0.50 1.50 4.50 94.1 ± 1.5 82.2 ± 4.1 8.4 18.9 29.5
Cycloate LOQ–502 y = 598248x − 1864 0.9974 ± 0.15 - 1.67 5.02 101.6 ± 6.7 101.3 ± 0.1 10.1 15.4 13.8
Hexaflumuron LOQ–419 y = 633012x − 654 0.9977 ± 1.28 - 1.40 4.19 81.8 ± 10.2 81.7 ± 1.3 5.6 14.7 41.0
Trifloxystrobin LOQ–432 y = 17415017x + 17609 0.9999 ± 0.27 0.70 1.44 4.32 96.7 ± 7.3 94.7 ± 2.0 7.6 8.4 17.1
Quizalofop-ethyl LOQ–398 y = 3145820x − 5888 0.9998 ± 0.18 0.40 1.33 3.98 100.8 ± 5.7 100.1 ± 1.5 11.3 5.4 11.8
Cycloxydim LOQ–407 y = 137254x + 708 0.9986 ± 0.01 1.50 1.36 4.07 85.2 ± 7.8 96.3 ± 0.8 14.2 12.1 30.9
Buprofezin LOQ–465 y = 20507228x + 51039 0.9998 ± 0.89 1.00 1.55 4.65 95.0 ± 8.0 93.9 ± 0.7 8.4 14.0 19.2
Tebufenpyrad LOQ–401 y = 4341528x + 15573 0.9994 ± 1.27 0.80 1.34 4.01 83.6 ± 6.8 81.7 ± 1.8 9.7 9.4 36.7
Emamectin Benzoate LOQ–522 y = 3632831x − 14712 0.9998 ± 0.25 0.02 1.74 5.22 98.8 ± 5.2 95.2 ± 3.1 12.4 7.4 13.7
Propaquizafop LOQ–431 y = 2547342x − 6777 0.9971 ± 0.02 0.05 1.44 4.31 99.6 ± 8.8 100.0 ± 2.5 15.4 16.1 18.1
Metaflumizone LOQ–410 y = 949238x − 6681 0.9983 ± 0.03 0.60 1.37 4.10 90.1 ± 3.8 75.6 ± 8.6 10.6 13.0 41.8
Oxadiazon LOQ–403 y = 726169x − 4189 0.9983 ± 0.05 0.05 1.34 4.03 94.3 ± 4.8 88.1 ± 0.4 8.4 8.4 21.4
Allethrin LOQ–649 y = 439397x − 5650 0.9963 ± 0.22 - 2.16 6.49 87.7 ± 4.3 81.2 ± 0.1 10.1 10.4 32.7
Piperonyl butoxide LOQ–404 y = 31536094x + 11745 0.9999 ± 0.01 - 1.35 4.04 104.8 ± 5.5 100.9 ± 1.8 5.6 9.7 14.6
Chlorpyriphos LOQ–395 y = 638457x − 2533 0.9992 ± 0.01 0.01 1.32 3.95 104.5 ± 5.1 109.5 ± 6.0 11.4 7.4 16.1
Hexythiazox LOQ–358 y = 10457257x − 49960 0.9987 ± 0.01 0.50 1.19 3.58 97.9 ± 5.8 97.1 ± 0.5 14.3 14.1 12.5
Pyriproxyfen LOQ–418 y = 6633898x − 13776 0.9994 ± 0.02 1.00 1.39 4.18 83.4 ± 4.8 77.7 ± 3.5 15.8 12.8 40.2
Pendimethalin LOQ–333 y = 1172935x − 2381 0.9999 ± 0.01 0.05 1.11 3.33 84.2 ± 6.3 81.0 ± 4.6 14.2 8.4 36.9
Flufenoxuron LOQ–391 y = 3953910x + 11436 0.9990 ± 0.48 0.50 * 1.30 3.91 81.9 ± 7.4 79.5 ± 1.5 9.7 9.5 40.7
Propargite LOQ–382 y = 6439838x + 13171 0.9997 ± 1.64 0.01 * 1.27 3.82 86.8 ± 6.0 81.8 ± 1.2 14.1 14.5 33.5
Lufenuron LOQ–437 y = 568999x + 552 0.9993 ± 0.09 0.50 1.46 4.37 93.5 ± 5.4 96.3 ± 0.6 7.5 12.3 15.7
Etoxazole LOQ–516 y = 393488x + 312 0.9998 ± 0.02 0.07 1.72 5.16 88.7 ± 6.6 83.2 ± 2.7 18.3 17.2 31.5
Fenpyroximate(E) LOQ–460 y = 24740316x + 67928 0.9987 ± 0.41 0.20 1.53 4.60 96.2 ± 8.0 95.2 ± 1.2 10.3 9.3 18.0
Deltamethrin LOQ–345 y = 212931x + 1529 0.9999 ± 0.01 0.07 1.15 3.45 96.8 ± 5.7 79.9 ± 1.1 4.8 10.3 36.0
Acrinathrin LOQ–475 y = 48200x − 207 0.9998 ± 0.27 0.10 1.58 4.75 89.9 ± 12.2 88.8 ± 10.7 5.4 8.3 34.6
Pyridaben LOQ–418 y = 18219756x + 7898 0.9999 ± 0.07 0.30 1.39 4.18 98.6 ± 2.6 88.7 ± 9.2 8.6 13.4 23.2
Tau–Fluvalinate LOQ–431 y = 17740157x − 22927 0.9999 ± 0.13 0.10 1.44 4.31 85.0 ± 11.4 94.2 ± 3.8 4.5 14.1 34.7
Fenarimol LOQ–444 y = 167645x + 140 0.9999 ± 0.57 0.02 * 1.48 4.44 84.2 ± 19.4 86.3 ± 10.2 11.1 5.6 48.7
Etofenprox LOQ–387 y = 5530818x + 37481 0.9981 ± 0.24 1.00 1.29 3.87 92.4 ± 5.6 93.3 ± 0.5 7.2 13.1 18.0
Bifenthrin LOQ–417 y = 39808x + 128 0.9989 ± 0.58 0.30 * 1.39 4.17 80.4 ± 12.6 76.2 ± 1.4 11.1 8.7 49.2
Famoxadone LOQ–376 y = 168731x − 107 1.0000 ± 0.07 2.00 1.25 3.76 91.7 ± 10.9 94.4 ± 7.1 8.7 9.8 27.6

* Pesticides not allowed in EU with an MRL on tomatoes.