Table 1.
Linearities, curves, LODs, and LOQs and method validation parameters for the analysis of 115 target a.i. in grapes juice, must and wine in LC-MS/MS.
| Pesticide | Linearity | Linear Regression Equation y | r2 ± RSD% y | MRL | LOD | LOQ | Apparent Recovery (%, n = 18) y | RSDr (3 × LOQ) y | RSDwR (3 × LOQ) y | U *,y | |
|---|---|---|---|---|---|---|---|---|---|---|---|
| (μg kg−1) | (mg kg−1) | (μg kg−1) | (μg kg−1) | LOQ | 5 × LOQ | n = 18 | n = 36 | ||||
| Cyromazine | LOQ—410 | y = 9,931,209.1x + 52,051.8 | 0.9998 ± 0.17 | 0.05 | 1.37 | 4.10 | 107.1 ± 12.9 | 100.1 ± 11.7 | 10.9 | 9.9 | 30.0 |
| Methamidophos | LOQ—410 | y = 4,887,931x + 119,357.3 | 0.9999 ± 0.05 | 0.01 | 1.37 | 4.10 | 99.4 ± 8.3 | 95.6 ± 6.8 | 11.8 | 11.5 | 23.3 |
| Acephate | LOQ—440 | y = 375,881x − 24,719.0 | 0.9969 ± 0.17 | 0.01 | 1.45 | 4.40 | 93.1 ± 18.3 | 92.7 ± 5.4 | 12.7 | 10.6 | 14.7 |
| Formetanate | LOQ—410 | y = 14,913,520x − 37,835.2 | 0.9998 ± 0.12 | 0.1 | 1.38 | 4.10 | 78.5 ± 9.9 | 77.6 ± 6.3 | 14.5 | 13.2 | 20.6 |
| Pymetrozine | LOQ—470 | y = 696,973x − 11,370.1 | 0.9976 ± 0.16 | 0.02 | 1.58 | 4.70 | 109.4 ± 11.7 | 99.7 ± 7.8 | 13.2 | 13.3 | 15.1 |
| Omethoate | LOQ—620 | y = 32,351x + 372 | 0.9997 ± 0.08 | 0.01 | 2.07 | 6.20 | 81.4 ± 6.5 | 86.1 ± 3.9 | 13.9 | 13.9 | 38.2 |
| Propamocarb | LOQ—420 | y = 43,247,201x − 8829 | 1.0000 ± 0.21 | 0.01 | 1.39 | 4.10 | 96.9 ± 9.7 | 94.1 ± 8.7 | 11.3 | 9.4 | 30.3 |
| Oxamyl | LOQ—400 | y = 5,159,083x − 5579 | 0.9999 ± 0.09 | 0.01 | 1.34 | 4.00 | 93.6 ± 4.1 | 82.9 ± 6.3 | 6.7 | 6.0 | 37.9 |
| Methomyl | LOQ—410 | y = 5,917,725x + 7746 | 1.0000 ± 0.10 | 0.01 | 1.37 | 4.10 | 109.1 ± 7.4 | 105.7 ± 10.3 | 10.4 | 9.2 | 31.0 |
| Flonicamid | LOQ—500 | y = 784,761x + 1544 | 0.9982 ± 0.10 | 0.03 | 1.31 | 5.00 | 90.4 ± 11.6 | 92.4 ± 5.9 | 13.4 | 14.4 | 13.7 |
| Thiamethoxam | LOQ—520 | y = 11,189,678x + 71,281 | 0.9972 ± 0.41 | 0.40 | 1.75 | 5.20 | 101.8 ± 11.3 | 100.9 ± 7.5 | 9.9 | 9.7 | 34.6 |
| Carbendazim | LOQ—400 | y = 5,329,930x + 3082 | 0.9996 ± 0.16 | 0.30 | 1.33 | 4.00 | 75.8 ± 9.7 | 80.1 ± 3.1 | 8.6 | 8.0 | 15.6 |
| Monocrotophos | LOQ—410 | y = 17,644,763x + 44,731 | 0.9984 ± 0.19 | 0.01 | 1.38 | 4.10 | 93.4 ± 4.1 | 85.6 ± 8.4 | 8.6 | 7.5 | 40.4 |
| Chlordimeform | LOQ—400 | y = 853,728x − 1979 | 1.0000 ± 0.14 | - | 1.32 | 4.00 | 81.9 ± 8.4 | 76.9 ± 10.7 | 12.8 | 13.5 | 13.7 |
| Cypermethrin | LOQ—410 | y = 5,132,597x + 20,901 | 0.9964 ± 0.12 | 0.50 * | 1.73 | 4.10 | 87.5 ± 10.1 | 85.4 ± 6.4 | 12.2 | 12.4 | 36.6 |
| Imidacloprid | LOQ—320 | y = 5,358,564x + 20,834 | 0.9999 ± 0.02 | 1.00 * | 1.07 | 3.20 | 100.9 ± 1.7 | 99.5 ± 5.2 | 5.4 | 4.8 | 12.6 |
| Methiocarb | LOQ—390 | y = 31,899,495x + 73,553 | 0.9977 ± 0.19 | 0.30 | 1.29 | 3.90 | 75.6 ± 9.9 | 81.4 ± 9.2 | 7.3 | 6.4 | 31.0 |
| Dimethoate | LOQ—410 | y = 9,144,917x + 45,650 | 0.9999 ± 0.21 | 0.01 | 1.36 | 4.10 | 103.5 ± 10.0 | 94.8 ± 4.7 | 8.4 | 7.2 | 33.4 |
| Acetamiprid | LOQ—400 | y = 13,742,437x + 39,503 | 0.9998 ± 0.43 | 0.50 * | 1.33 | 4.00 | 94.2 ± 3.7 | 89.7 ± 3.8 | 10.3 | 11.3 | 24.3 |
| Cymoxanil | LOQ—440 | y = 7,081,921x + 5097 | 0.9973 ± 0.34 | 0.30 * | 1.45 | 4.40 | 97.5 ± 6.8 | 83.5 ± 7.8 | 13.1 | 12.2 | 35.2 |
| Thiacloprid | LOQ—440 | y = 4,714,164x + 21,318 | 0.9997 ± 0.26 | 0.01 | 1.46 | 4.40 | 104.7 ± 9.7 | 100.9 ± 9.2 | 12 | 11.6 | 29.1 |
| Atrazine-desethyl | LOQ—430 | y = 8,730,484x + 17,192 | 0.9994 ± 0.18 | - | 1.43 | 4.30 | 100.9 ± 6.2 | 98.7 ± 5.8 | 9.9 | 9.1 | 12.3 |
| Aldicarb | LOQ—460 | y = 22,774x − 3 | 0.9996 ± 0.42 | 0.02 | 1.53 | 4.60 | 97.5 ± 10.2 | 91.4 ± 6.2 | 9.1 | 9.5 | 32.4 |
| Pirimicarb | LOQ—410 | y = 30,848,679x + 25,212 | 0.9997 ± 0.16 | 0.01 * | 1.37 | 4.10 | 103.1 ± 7.6 | 100.9 ± 11.8 | 8.6 | 9.0 | 15.6 |
| Dichlorvos | LOQ—410 | y = 450,147x + 175 | 1.0000 ± 0.17 | 0.01 | 1.37 | 4.10 | 81.9 ± 8.3 | 79.5 ± 6.0 | 12.9 | 10.8 | 17.5 |
| Thiophanate-methyl | LOQ—410 | y = 17,268,518x − 53,036 | 0.9993 ± 0.30 | 3.00 * | 1.35 | 4.10 | 94.6 ± 15.0 | 91.7 ± 7.6 | 13.0 | 15.5 | 21.2 |
| Metribuzin | LOQ—430 | y = 3,761,325x + 17,279 | 0.9998 ± 0.47 | 0.10 * | 1.42 | 4.30 | 93.7 ± 17.7 | 103.7 ± 4.4 | 9.0 | 7.3 | 20.5 |
| Carbofuran | LOQ—420 | y = 27,252,840x + 33,458 | 0.9990 ± 0.56 | 0.002 | 1.39 | 4.20 | 91.8 ± 9.9 | 90.9 ± 6.5 | 8.1 | 8.3 | 21.2 |
| Carbaryl | LOQ—410 | y = 14,046,644x + 7098 | 0.9972 ± 0.28 | 0.01 | 1.37 | 4.10 | 115.9 ± 8.0 | 99.7 ± 9.1 | 9.9 | 9.1 | 47.6 |
| Imazalil | LOQ—430 | y = 972,258x + 947 | 0.9995 ± 0.19 | 0.01 * | 1.44 | 4.30 | 75.8 ± 3.2 | 75.9 ± 4.2 | 14.8 | 13.9 | 29.6 |
| Fosthiazate | LOQ—400 | y = 720,338x + 1656 | 0.9997 ± 0.05 | 0.02 * | 1.32 | 4.00 | 94.1 ± 6.1 | 91.8 ± 8.1 | 9.1 | 8.2 | 20.8 |
| Disulfoton-Sulfoxide | LOQ—470 | y = 12,702,349x + 19,964 | 0.9999 ± 0.65 | - | 1.57 | 4.70 | 107.4 ± 9.0 | 101.9 ± 6.2 | 10.5 | 7.5 | 19.9 |
| Flutriafol | LOQ—500 | y = 3625x + 183 | 0.9982 ± 0.01 | 1.50 * | 1.57 | 5.00 | 99.4 ± 11.1 | 97.5 ± 4.0 | 13.8 | 14.5 | 39.0 |
| Metalaxyl | LOQ—390 | y = 4371x + 183 | 0.9991 ± 0.19 | 1.00 * | 1.30 | 3.90 | 78.9 ± 8.9 | 75.9 ± 6.1 | 9.8 | 9.6 | 26.6 |
| Methidathion | LOQ—420 | y = 396,329x − 101 | 0.9970 ± 0.10 | 0.02 | 1.41 | 4.20 | 96.7 ± 9.4 | 90.7 ± 8.9 | 11.5 | 9.4 | 30.4 |
| Pyrimethanil | LOQ—390 | y = 1,208,059x − 4250 | 0.9998 ± 0.06 | 5.00 * | 1.32 | 3.90 | 101.6 ± 7.5 | 99.8 ± 4.3 | 10.6 | 10.4 | 15.9 |
| Azinphos-methyl | LOQ—460 | y = 398,216x + 390 | 0.9998 ± 0.46 | 0.05 | 1.55 | 4.60 | 99.4 ± 4.9 | 91.7 ± 9.3 | 13.9 | 11.2 | 20.9 |
| Chlorantraniliprole | LOQ—400 | y = 585,240x + 2 | 0.9991 ± 0.32 | 1.00 * | 1.33 | 4.00 | 87.5 ± 3.8 | 85.4 ± 7.5 | 11.5 | 9.4 | 19.5 |
| Diethofencarb | LOQ—390 | y = 17,914,008x +75,801 | 0.9993 ± 0.78 | 0.90 | 1.28 | 3.90 | 95.9 ± 10.2 | 91.8 ± 3.6 | 13.2 | 9.9 | 37.6 |
| Azoxystrobin | LOQ—430 | y = 37027632 + 20,546 | 0.9981 ± 0.39 | 3.00 * | 1.44 | 4.30 | 100.8 ± 8.5 | 97.6 ± 9.2 | 10.9 | 8.6 | 39.0 |
| Propanil | LOQ—490 | y = 1,172,102x − 4083 | 0.9998 ± 0.15 | 0.01 | 1.31 | 4.90 | 91.7 ± 4.1 | 89.9 ± 7.8 | 12.7 | 12.6 | 28.0 |
| Fenamidone | LOQ—390 | y = 19,532,597x + 43,718 | 1.0000 ± 1.00 | 0.60 | 1.30 | 3.90 | 96.8 ± 3.5 | 94.7 ± 10.3 | 9.5 | 9.1 | 24.7 |
| Diclobutrazol | LOQ—390 | y = 145,538x + 476 | 0.9988 ± 0.27 | - | 1.30 | 3.90 | 99.8 ± 10.7 | 98.4 ± 5.2 | 11.9 | 10.6 | 34.1 |
| Boscalid | LOQ—410 | y = 4,252,887x + 877 | 0.9995 ± 0.46 | 5.00 * | 1.36 | 4.10 | 104.5 ± 5.6 | 101.7 ± 9.3 | 14.8 | 14.4 | 24.4 |
| Dimethomorph | LOQ—390 | y = 14,639,124x + 39,105 | 0.9989 ± 0.51 | 3.00 * | 1.31 | 3.90 | 93.8 ± 7.4 | 90.7 ± 7.5 | 10.2 | 7.9 | 24.1 |
| Benthiavalicarb | LOQ—240 | y = 4,160,577x + 5366 | 0.9998 ± 0.23 | 0.30 * | 0.78 | 2.40 | 111.4 ± 6.8 | 104.8 ± 3.9 | 8.8 | 8.8 | 25.4 |
| Mandipropamid | LOQ—460 | y = 5,148,550x − 20,963 | 0.9998 ± 0.78 | 2.00 * | 1.52 | 4.60 | 85.6 ± 1.9 | 80.9 ± 5.4 | 10.0 | 10.6 | 31.5 |
| Molinate | LOQ—620 | y = 47,567x − 140 | 0.9999 ± 0.58 | 0.01 | 2.07 | 6.20 | 92.2 ± 7.1 | 93.7 ± 9.6 | 14.7 | 12.7 | 19.2 |
| Chloroxuron | LOQ—430 | y = 12,252,052x − 45,885 | 0.9997 ± 0.91 | 0.01 | 1.42 | 4.30 | 105.7 ± 9.7 | 99.4 ± 7.4 | 10.6 | 10.1 | 28.5 |
| Bifenazate | LOQ—400 | y = 1,008,299x + 76,836 | 0.9983 ± 0.47 | 0.70 * | 1.33 | 4.00 | 87.0 ± 4.1 | 85.4 ± 4.6 | 11.7 | 9.9 | 29.8 |
| Triadimenol | LOQ—500 | y = 3,828,694x + 27.482 | 0.9989 ± 1.67 | 0.30 | 1.65 | 5.00 | 84.9 ± 7.3 | 90.7 ± 9.1 | 7.5 | 6.0 | 22.0 |
| Cyproconazole | LOQ—410 | y = 14,106,016x + 110,236 | 0.9980 ± 0.15 | 0.02 * | 1.37 | 4.10 | 109.2 ± 6.2 | 110.7 ± 7.1 | 12.4 | 9.4 | 40.3 |
| Iprovalicarb | LOQ—410 | y = 4,408,560x + 40,826 | 0.9999 ± 0.19 | 2.00 * | 1.36 | 4.10 | 90.6 ± 10.0 | 94.5 ± 6.4 | 13.5 | 13.8 | 29.9 |
| Fenhexamid | LOQ—440 | y = 3,699,942x + 18,108 | 0.9975 ± 1.00 | 15.00 * | 1.45 | 4.40 | 112.4 ± 9.9 | 100.7 ± 4.6 | 10.5 | 8.0 | 13.2 |
| Azinphos-ethyl | LOQ—390 | y = 367,433x + 492 | 0.9976 ± 0.49 | 0.02 | 1.30 | 3.90 | 79.8 ± 5.5 | 75.9 ± 9.5 | 12.0 | 10.2 | 14.4 |
| Myclobutanil | LOQ—410 | y = 123,049x − 122 | 0.9994 ± 0.24 | 1.50* | 1.37 | 4.10 | 78.5 ± 9.1 | 86.1 ± 3.7 | 10.6 | 9.1 | 39.1 |
| Tetraconazole | LOQ—520 | y = 9,182,219x − 30,061 | 0.9994 ± 0.17 | 0.50 * | 1.72 | 5.20 | 109.7 ± 6.4 | 99.8 ± 7.9 | 11.5 | 9.5 | 38.8 |
| Bupirimate | LOQ—400 | y = 7,147,770x + 5118 | 0.9992 ± 0.54 | 1.50 * | 1.32 | 4.00 | 99.4 ± 14.5 | 94.3 ± 9.2 | 10.9 | 7.1 | 26.1 |
| Spirotetramat | LOQ—500 | y = 2,820,842x + 73,839 | 0.9980 ± 0.92 | 2.00 * | 1.68 | 5.00 | 81.8 ± 3.6 | 78.5 ± 7.7 | 16.2 | 14.5 | 39.2 |
| Flufenacet | LOQ—410 | y = 10,522,988x + 50,386 | 0.9981 ± 0.67 | 0.05 * | 1.38 | 4.10 | 89.7 ± 4.6 | 86.7 ± 6.4 | 13.7 | 12.0 | 28.1 |
| Mepanipyrim | LOQ—410 | y = 328,904x − 348 | 0.9975 ± 1.01 | 2.00 * | 1.36 | 4.10 | 99.4 ± 10.1 | 95.4 ± 4.6 | 12.1 | 8.7 | 35.4 |
| Ethoprop | LOQ—380 | y = 5,056,608x + 20,031 | 0.9972 ± 2.08 | - | 1.26 | 3.80 | 92.6 ± 5.1 | 96.7 ± 3.2 | 12.6 | 11.5 | 31.3 |
| Napropamide | LOQ—410 | y = 6,724,980x + 62,380 | 0.9969 ± 0.41 | 0.01 * | 1.38 | 4.10 | 104.8 ± 6.2 | 103.4 ± 9.1 | 12.9 | 12.6 | 24.2 |
| Cyazofamid | LOQ—410 | y = 54,070x + 229 | 0.9988 ± 0.30 | 2.00 * | 1.35 | 4.10 | 103.9 ± 11.0 | 98.9 ± 7.2 | 9.2 | 7.4 | 16.3 |
| Cyprodinil | LOQ—410 | y = 2,997,671x + 13,504 | 0.9994 ± 0.12 | 3.00 * | 1.36 | 4.10 | 98.7 ± 5.1 | 97.1 ± 8.9 | 9.6 | 9.2 | 19.4 |
| Flusilazole | LOQ—460 | y = 9,842,141x + 54,831 | 0.9992 ± 0.85 | 0.01 | 1.52 | 4.60 | 110.1 ± 4.2 | 100.7 ± 6.2 | 11.1 | 9.8 | 27.8 |
| Fenamiphos | LOQ—550 | y = 2,610,314x + 116,029 | 0.9987 ± 0.24 | 0.03 * | 1.82 | 5.50 | 99.7 ± 9.1 | 96.4 ± 4.2 | 11.6 | 8.1 | 24.7 |
| Aclonifen | LOQ—390 | y = 96,057x + 89 | 0.9967 ± 0.39 | 0.01 * | 1.31 | 3.90 | 97.1 ± 6.2 | 99.1 ± 6.7 | 13.4 | 12.3 | 4.9 |
| Penconazole | LOQ—400 | y = 6,090,424x + 15,097 | 0.9963 ± 0.76 | 0.50 * | 1.33 | 4.00 | 101.7 ± 4.2 | 99.7 ± 3.1 | 10.3 | 8.0 | 31.9 |
| Tebuconazole | LOQ—400 | y = 19,544,180x + 77,610 | 0.9984 ± 1.05 | 1.00* | 1.34 | 4.00 | 99.5 ± 6.1 | 89.4 ± 7.1 | 8.9 | 7.1 | 20.5 |
| Iprodione | LOQ—460 | y = 82,937x + 89 | 0.9966 ± 0.64 | 0.01 | 1.52 | 4.60 | 93.4 ± 2.0 | 97.4 ± 9.2 | 12.8 | 11.3 | 17.6 |
| Benalaxyl | LOQ—480 | y = 23,788,991x + 92,142 | 0.9958 ± 0.87 | 0.30 * | 1.60 | 4.80 | 100.0 ± 1.9 | 99.2 ± 6.1 | 9.0 | 8.4 | 48.2 |
| Zoxamide | LOQ—410 | y = 5,772,043x + 12,727 | 0.9984 ± 0.21 | 5.00 * | 1.37 | 4.10 | 98.7 ± 6.4 | 99.0 ± 2.8 | 12.4 | 12.4 | 34.4 |
| Spinosyn A | LOQ—430 | y = 1,125,007x − 3076 | 0.9986 ± 0.54 | 0.50 * | 1.44 | 4.30 | 75.6 ± 8.1 | 79.4 ± 7.6 | 10.2 | 9.6 | 36.6 |
| Pyraclostrobin | LOQ—420 | y = 13,354,734x − 5243 | 0.9968 ± 1.09 | 2.00 * | 1.39 | 4.20 | 90.8 ± 10.2 | 95.1 ± 9.9 | 15.3 | 15.2 | 32.9 |
| Cyflufenamid | LOQ—410 | y = 5,945,864x + 38,431 | 0.9989 ± 0.45 | - | 1.36 | 4.10 | 81.9 ± 1.6 | 91.1 ± 4.1 | 8.7 | 7.9 | 28.4 |
| Clofentezin | LOQ—410 | y = 1,910,622x −533 | 0.9990 ± 0.73 | 1.00 * | 1.36 | 4.10 | 85.7 ± 9.4 | 101.7 ± 10.8 | 9.1 | 9.0 | 23.9 |
| Bitertanol | LOQ—410 | y = 6,031,192x + 40,609 | 0.9988 ± 0.29 | 0.01 | 1.35 | 4.10 | 101.9 ± 6.7 | 99.7 ± 6.9 | 15.0 | 15.2 | 49.3 |
| Phosalone | LOQ—580 | y = 6,702,437x + 16,186 | 0.9970 ± 0.13 | 0.01 | 1.93 | 5.80 | 98.7 ± 4.4 | 91.7 ± 9.1 | 14.8 | 15.6 | 38.1 |
| Metrafenone | LOQ—470 | y = 9,239,760x + 20,728 | 0.9975 ± 0.56 | 7.00 * | 1.56 | 4.70 | 99.1 ± 8.9 | 89.1 ± 7.9 | 12.9 | 12.0 | 33.9 |
| Difenconazole | LOQ—490 | y = 20,779,327x + 20,116 | 0.9974 ± 0.89 | 3.00 * | 1.62 | 4.90 | 96.7 ± 2.3 | 91.7 ± 3.8 | 10.7 | 8.2 | 33.5 |
| Chlorpyrifos-methyl | LOQ—410 | y = 65,820x − 225 | 0.9974 ± 0.34 | 0.01 | 1.38 | 4.10 | 94.8 ± 3.9 | 99.6 ± 8.3 | 17.9 | 17.6 | 26.7 |
| Ametoctradin | LOQ—320 | y = 8,626,247x + 1875 | 0.9962 ± 0.46 | 6.00 * | 1.06 | 3.20 | 99.7 ± 9.1 | 97.8 ± 10.4 | 8.5 | 8.7 | 31.9 |
| Spinosyn D | LOQ—430 | y = 209,477x − 615 | 0.9971 ± 0.24 | 0.50 * | 1.44 | 4.30 | 89.5 ± 4.6 | 85.4 ± 6.1 | 8.1 | 5.7 | 39.1 |
| Indoxacarb | LOQ—450 | y = 1,790,071x − 2915 | 0.9993 ± 0.76 | 2.00 * | 1.50 | 4.50 | 97.4 ± 9.5 | 91.6 ± 9.1 | 7.0 | 6.3 | 40.1 |
| Cycloate | LOQ—500 | y = 598,248x − 1864 | 0.9973 ± 0.50 | - | 1.67 | 5.00 | 106.9 ± 2.7 | 100.1 ± 3.1 | 9.1 | 10.9 | 36.9 |
| Hexaflumuron | LOQ—420 | y = 633,012x − 654 | 0.9985 ± 0.94 | - | 1.40 | 4.20 | 78.5 ± 15.2 | 79.4 ± 9.3 | 9.7 | 9.8 | 37.9 |
| Trifloxystrobin | LOQ—430 | y = 17,415,017x + 17,609 | 0.9956 ± 0.34 | 3.00 * | 1.44 | 4.30 | 91.9 ± 4.3 | 95.9 ± 10.0 | 10.2 | 9.6 | 35.3 |
| Quizalofop-ethyl | LOQ—400 | y = 3,145,820x − 5888 | 0.9955 ± 0.78 | 0.02 * | 1.33 | 4.00 | 102.4 ± 3.7 | 99.4 ± 11.5 | 13.5 | 10.8 | 44.4 |
| Metaflumizone | LOQ—410 | y = 949,238x − 6681 | 0.9971 ± 0.60 | 0.05 * | 1.37 | 4.10 | 95.6 ± 6.8 | 96.1 ± 4.6 | 8 | 7.8 | 48.3 |
| Buprofezin | LOQ—470 | y = 20,507,228x + 51,039 | 0.9999 ± 0.24 | 0.01 * | 1.55 | 4.70 | 93.4 ± 9.0 | 97.2 ± 9.7 | 12.7 | 11.4 | 21.7 |
| Tebufenpyrad | LOQ—400 | y = 4,341,528x + 15,573 | 0.9987 ± 0.53 | 0.60 * | 1.34 | 4.00 | 80.9 ± 7.8 | 78.9 ± 6.8 | 13.6 | 11.0 | 46.7 |
| Emamectin Benzoate | LOQ—520 | y = 3,632,831x − 14,712 | 0.9985 ± 0.25 | 0.05 * | 1.74 | 5.20 | 96.4 ± 11.2 | 98.1 ± 7.1 | 10.1 | 7.8 | 42.8 |
| Propaquizafop | LOQ—430 | y = 2,547,342x − 6777 | 0.9963 ± 0.12 | 0.02 * | 1.44 | 4.30 | 96.8 ± 3.8 | 100.6 ± 8.5 | 13.1 | 13.6 | 47.5 |
| Lufenuron | LOQ—440 | y = 568,999x + 552 | 0.9998 ± 1.02 | 0.01 * | 1.46 | 4.40 | 90.1 ± 9.4 | 94.9 ± 6.6 | 8.3 | 9.8 | 30.7 |
| Oxadiazon | LOQ—400 | y = 726,169x − 4189 | 0.9973 ± 0.98 | 0.05 | 1.34 | 4.00 | 91.7 ± 7.8 | 90.7 ± 5.4 | 9.9 | 11.1 | 35.9 |
| Allethrin | LOQ—650 | y = 439,397x − 5650 | 0.9999 ± 0.01 | - | 2.16 | 6.50 | 88.4 ± 10.3 | 79.1 ± 6.1 | 11.2 | 9.8 | 15.5 |
| Piperonyl butoxide | LOQ—400 | y = 31,536,094x + 11,745 | 0.9988 ± 0.28 | - | 1.35 | 4.00 | 105.7 ± 9.5 | 99.8 ± 4.8 | 11.8 | 11.2 | 32.0 |
| Pyriproxyfen | LOQ—420 | y = 6,633,898x − 13,776 | 0.9981 ± 0.85 | 0.05 * | 1.39 | 4.20 | 80.9± 7.8 | 85.4 ± 9.5 | 9.5 | 9.6 | 25.4 |
| Cycloxydim | LOQ—410 | y = 137,254x + 708 | 0.9987 ± 0.57 | 0.50 * | 1.36 | 4.10 | 87.1 ± 3.8 | 87.4 ± 7.8 | 15.7 | 15.8 | 40.2 |
| Chlorpyriphos | LOQ—400 | y = 638,457x − 2533 | 0.9981 ± 0.64 | 0.01 | 1.32 | 4.00 | 101.9 ± 8.1 | 96.7 ± 3.0 | 10.2 | 10.8 | 24.7 |
| Hexythiazox | LOQ—360 | y = 10,457,257x − 49,960 | 0.9985 ± 0.95 | 1.00 * | 1.19 | 3.60 | 95.7 ± 9.8 | 100.5 ± 5.5 | 9.9 | 8.7 | 42.4 |
| Pendimethalin | LOQ—330 | y = 1,172,935x − 2381 | 0.9978 ± 0.46 | 0.05 * | 1.11 | 3.30 | 87.6 ± 10.3 | 89.1 ± 8.6 | 8.4 | 8.4 | 20.6 |
| Flufenoxuron | LOQ—390 | y = 3,953,910x + 11,436 | 0.9984 ± 0.30 | 2.00 | 1.30 | 3.90 | 83.7 ± 3.4 | 79.7 ± 9.5 | 7.6 | 6.6 | 29.1 |
| Propargite | LOQ—380 | y = 6,439,838x + 13,171 | 0.9976 ± 0.76 | 0.01 | 1.27 | 3.80 | 81.8 ± 5.0 | 79.1 ± 4.2 | 14.3 | 15.5 | 27.8 |
| Fenpyroximate(E) | LOQ—460 | y = 24,740,316x + 67,928 | 0.9979 ± 0.12 | 0.30 * | 1.53 | 4.60 | 99.8 ± 4.0 | 98.7 ± 6.2 | 9.4 | 10.4 | 27.3 |
| Deltamethrin | LOQ—340 | y = 212,931x + 1529 | 0.9976 ± 0.54 | 0.05 | 1.15 | 3.40 | 94.5 ± 9.7 | 93.4 ± 8.1 | 14.2 | 14.2 | 21.0 |
| Acrinathrin | LOQ—470 | y = 48,200x − 207 | 0.9972 ± 0.56 | 0.10 * | 1.58 | 4.70 | 79.4 ± 10.2 | 80.9 ± 3.7 | 11.3 | 12.7 | 31.2 |
| Etoxazole | LOQ—520 | y = 393,488x + 312 | 0.9969 ± 0.75 | 0.50 * | 1.72 | 5.20 | 90.7 ± 9.6 | 95.7 ± 7.7 | 9.6 | 9.6 | 36.5 |
| Pyridaben | LOQ—420 | y = 18,219,756x + 7898 | 0.9966 ± 0.32 | 0.01 * | 1.39 | 4.20 | 99.8 ± 5.6 | 94.7 ± 8.2 | 14.3 | 14.2 | 22.5 |
| Tau—Fluvalinate | LOQ—430 | y = 17,740,157x − 22,927 | 0.9993 ± 0.46 | 1.00 * | 1.44 | 4.30 | 100.8 ± 1.4 | 102.5 ± 6.8 | 17.7 | 18.0 | 22.9 |
| Fenarimol | LOQ—440 | y = 167,645x + 140 | 0.9971 ± 0.92 | 0.30 | 1.48 | 4.40 | 83.9 ± 6.4 | 89.8 ± 7.2 | 9.8 | 10.0 | 45.3 |
| Etofenprox | LOQ—390 | y = 5,530,818x + 37,481 | 0.9993 ± 0.15 | 4.00 * | 1.29 | 3.90 | 97.1 ± 8.6 | 95.4 ± 9.5 | 7.5 | 6.1 | 17.5 |
| Bifenthrin | LOQ—420 | y = 39,808x + 128 | 0.9977 ± 1.46 | 0.30 | 1.39 | 4.20 | 89.1 ± 4.6 | 86.1 ± 11.4 | 6.8 | 6.1 | 20.0 |
| Famoxadone | LOQ—380 | y = 168,731x − 107 | 0.9984 ± 0.12 | 2.00 * | 1.25 | 3.80 | 89.5 ± 8.9 | 82.8 ± 4.1 | 11.0 | 9.8 | 49.1 |
* Pesticides allowed in EU with an MRL on wine grapes. y validation data (linear regression equation, r2, Apparent recovery, RSDr and RSDwr, and U) represent the average values from grape juice, must and wine.