GC-MS/MSによる食品中残留農薬の定量分析 -ほうれん草抽出液中農薬の定量分析-
MSTips No.261
今日『食の安全』は世界的な規模で取り組むべき重要な課題であり、各国においては食品中残留農薬の基準値を設定し、独自の残留農薬規制を策定している。日本では平成18年5月末日にポジティブリスト制が施行されたが、人の健康を損なう恐れのない量、いわゆる一律基準としては10ppbが採用されている。ポジティブリスト制により測定対象農薬数は増え、食品中の残留農薬を精度良く、且つ一斉に分析可能な手法が求められている。質量分析計（MS）は検出感度が高い特長を有しているが、その中でも特に感度と選択性に優れたMS/MS法が農薬分析の主流となりつつある。
JMS-TQ4000GCはMS/MSのコリジョンセルに独自のイオン蓄積/排出機構を備え、また新規開発したファームウェアにより最大36,000トランジションによるMS/MS測定が可能な最新のGC-MS/MSである。今回、JMS-TQ4000GCを用いて、ほうれん草抽出液に添加した農薬成分の定量分析を実施したので報告する。
測定条件
標準溶液の調整には富士フイルム和光純薬株式会社製の農薬混合標準液PLシリーズを用いた。PL1、2、3、4、5、6、11、12を等量混合したものを準備し、それを段階的に希釈して1、5、10、50、100ppbの標準溶液を作製した。また、Analyte Protectants にはPEG300を用いた。
測定試料はほうれん草15gをAOAC法で処理して得た抽出液と標準溶液100ppbを9:1で混合したものを用いた。今回は150成分の農薬について定量分析を実施した。今回使用した測定条件をTable1に示す。
GC-MS/MS, JMS-TQ4000GC
Table1 Measurement condition
[GC-TQMS condition]
| System | JMS-TQ4000GC (JEOL) |
| Ionization mode | EI+: 70eV, 50µA |
| GC column | VF-5ms, 30m × 0.25mm, 0.25µm |
| Oven temp. | 50°C (1min) → 25°C/min → 125°C →10°C/min → 300°C |
| Inlet temp. | 250°C |
| Inlet mode | Splitless, 2µL |
| He flow | 1.0mL/min (Constant Flow) |
| MS/MS mode | Peak Dependent SRM |
結果
得られた測定結果の中から、4成分の農薬のSRMクロマトグラムをFig.1に示す。上段がほうれん草抽出液のみのデータで、下段が農薬を添加したほうれん草抽出液のデータである。MS/MS法の高選択性により、ほうれん草抽出液中の夾雑成分の影響を受けることなく農薬成分を検出できることを確認した。Table2には、農薬150成分の定量値（n=5）とその再現性（CV）を示す。既報MSTips260の人参抽出液における結果と比べると、定量値7~12ppb（回収率70~120%）、CV10%以下を達成した農薬数は若干減少していた。多くの農薬においては良好な結果が得られており、JMS-TQ4000GCが農薬分析に有効であることを確認した。
Fig.1 SRM chromatograms,
upper: Spinach extract solution only, lower: 10ppb pesticides in the spinach extract solution
Table 2 Quantitative result 150 pesticides in the spinach extract solution (n=5)
| No. | Compound | RT (min) | Quantitative values (ppb) | Ave. (ppb) | CV(%) | ||||
|---|---|---|---|---|---|---|---|---|---|
| No.1 | No.2 | No.3 | No.4 | No.5 | |||||
|
1 |
Atrazine |
12.37 | 10.0 | 10.0 | 9.7 | 10.4 | 9.2 | 9.9 | 4.4 |
|
2 |
Benthiocarb |
14.68 | 10.1 | 10.7 | 11.6 | 11.5 | 10.8 | 10.9 | 5.8 |
|
3 |
cis-Permethrin |
20.68 | 12.5 | 12.8 | 12.8 | 12.3 | 12.6 | 12.6 | 1.9 |
| 4 | Diflufenican | 18.31 | 11.7 | 11.6 | 12.0 | 11.2 | 10.7 | 11.4 | 4.3 |
| 5 | Fenamiphos | 16.24 | 9.1 | 11.6 | 10.4 | 10.9 | 9.5 | 10.3 | 9.8 |
| 6 | Fenarimol | 20.20 | 11.1 | 11.1 | 11.1 | 11.3 | 11.1 | 11.1 | 0.7 |
| 7 | Fenpropimorph | 14.74 | 11.0 | 11.4 | 10.7 | 11.8 | 10.6 | 11.1 | 4.6 |
| 8 | Norflurazon | 17.94 | 10.7 | 10.2 | 10.6 | 10.2 | 10.7 | 10.5 | 2.3 |
| 9 | Oxadiazon | 16.50 | 10.6 | 9.9 | 11.0 | 10.8 | 10.3 | 10.5 | 4.0 |
| 10 | Penconazole | 15.45 | 11.7 | 10.8 | 10.9 | 11.3 | 11.2 | 11.2 | 3.0 |
| 11 | Pendimethalin | 15.29 | 12.9 | 11.7 | 12.3 | 11.9 | 12.5 | 12.3 | 3.7 |
| 12 | Procymidone | 15.70 | 10.6 | 10.8 | 12.4 | 9.4 | 9.7 | 10.6 | 11.2 |
| 13 | Spiroxamine 1 | 13.78 | 8.6 | 8.3 | 8.2 | 8.6 | 8.5 | 8.4 | 2.1 |
| 14 | Spiroxamine 2 | 14.31 | 9.2 | 8.7 | 9.0 | 9.4 | 8.5 | 9.0 | 3.9 |
| 15 | Tefluthrine | 12.92 | 10.2 | 9.9 | 10.3 | 10.5 | 10.1 | 10.2 | 2.2 |
| 16 | Terbufos | 12.63 | 8.3 | 7.9 | 7.9 | 8.7 | 7.6 | 8.1 | 5.0 |
| 17 | Terbutryn | 14.31 | 10.5 | 9.6 | 10.1 | 10.4 | 9.7 | 10.0 | 4.0 |
| 18 | trans-Permethrin | 20.68 | 12.5 | 12.8 | 12.8 | 12.3 | 12.6 | 12.6 | 1.9 |
| 19 | Alachlor | 13.84 | 9.7 | 9.0 | 8.9 | 9.3 | 8.7 | 9.1 | 4.5 |
| 20 | Buprofezin | 16.68 | 11.2 | 11.7 | 11.1 | 11.9 | 11.9 | 11.6 | 3.2 |
| 21 | cis-Chlorfenvinphos | 15.49 | 6.3 | 7.6 | 7.9 | 7.6 | 6.4 | 7.2 | 10.4 |
| 22 | Cyproconazole 1 | 17.03 | 12.1 | 12.4 | 11.2 | 9.9 | 12.2 | 11.6 | 9.1 |
| 23 | Cyproconazole 2 | 17.03 | 11.6 | 11.0 | 12.0 | 12.3 | 11.3 | 11.7 | 4.6 |
| 24 | Difenoconazole 1 | 23.10 | 11.3 | 11.2 | 11.3 | 11.0 | 11.3 | 11.2 | 1.4 |
| 25 | Difenoconazole 2 | 23.18 | 11.7 | 11.1 | 11.2 | 11.3 | 11.4 | 11.3 | 2.0 |
| 26 | Ethion | 17.34 | 10.2 | 10.6 | 10.9 | 10.0 | 9.9 | 10.3 | 4.0 |
| 27 | Fenitrothion | 14.33 | 8.3 | 9.0 | 10.7 | 9.3 | 9.1 | 9.3 | 9.5 |
| 28 | Fenthion | 14.73 | 8.9 | 10.0 | 8.7 | 9.4 | 8.4 | 9.1 | 7.1 |
| 29 | Fluridone | 22.18 | 11.1 | 12.0 | 12.0 | 11.7 | 11.6 | 11.7 | 3.3 |
| 30 | Hexazinone | 18.24 | 9.5 | 9.9 | 10.0 | 9.5 | 9.0 | 9.6 | 3.9 |
| 31 | Isofenphos oxon | 14.79 | 10.1 | 12.8 | 13.3 | 10.4 | 10.6 | 11.5 | 12.9 |
| 32 | Isophenphos | 15.43 | 9.7 | 8.5 | 10.0 | 9.8 | 10.1 | 9.6 | 6.5 |
| 33 | Isoprothiolane | 16.44 | 11.1 | 11.2 | 11.1 | 10.1 | 12.4 | 11.2 | 7.4 |
| 34 | Propargite 1 | 18.31 | 6.7 | 7.2 | 7.4 | 7.0 | 7.3 | 7.1 | 4.1 |
| 35 | Propargite 2 | 18.31 | 6.9 | 7.3 | 7.4 | 7.2 | 6.8 | 7.1 | 3.9 |
| 36 | Propiconazole 1 | 17.93 | 12.6 | 12.9 | 12.2 | 12.1 | 12.0 | 12.4 | 3.1 |
| 37 | Propiconazole 2 | 18.07 | 13.5 | 12.4 | 12.3 | 12.9 | 13.0 | 12.8 | 4.0 |
| 38 | Propyzamide | 12.73 | 11.0 | 10.6 | 11.1 | 10.4 | 10.4 | 10.7 | 3.2 |
| 39 | Pyriproxyfen | 19.72 | 11.0 | 10.9 | 10.9 | 11.1 | 10.7 | 10.9 | 1.3 |
| 40 | trans-Chlorfenvinphos | 15.25 | 7.6 | 9.4 | 8.4 | 8.5 | 6.4 | 8.1 | 14.1 |
| 41 | Triadimenol 1 | 15.7 | 12.2 | 10.0 | 10.5 | 10.5 | 10.5 | 10.7 | 8.1 |
| 42 | Triadimenol 2 | 15.84 | 12.8 | 10.6 | 11.9 | 10.7 | 11.0 | 11.4 | 8.1 |
| 43 | Triallate | 13.13 | 7.4 | 7.9 | 8.1 | 8.3 | 7.4 | 7.8 | 5.0 |
| 44 | Vinclozoline | 13.76 | 7.2 | 8.0 | 8.3 | 7.5 | 7.6 | 7.7 | 5.6 |
| 45 | Acetamiprid | 18.92 | 10.3 | 10.9 | 10.7 | 10.3 | 11.5 | 10.8 | 4.8 |
| 46 | Allethrin 1 | 15.43 | 10.0 | 9.5 | 11.3 | 10.9 | 11.7 | 10.7 | 8.5 |
| 47 | Allethrin 2 | 15.51 | 9.0 | 10.5 | 9.2 | 9.1 | 10.3 | 9.6 | 7.7 |
| 48 | Bitertanol 1 | 20.66 | 14.1 | 14.1 | 14.0 | 14.1 | 14.0 | 14.0 | 0.5 |
| 49 | Bitertanol 2 | 20.76 | 10.8 | 11.1 | 11.0 | 11.7 | 11.2 | 11.2 | 3.0 |
| 50 | Bromopropylate | 19.00 | 9.6 | 10.6 | 10.7 | 10.3 | 9.8 | 10.2 | 4.7 |
| 51 | Chlorobenzilate | 17.19 | 8.7 | 9.4 | 10.1 | 9.4 | 8.6 | 9.3 | 6.9 |
| 52 | Chlorpyrifos | 14.63 | 8.5 | 9.4 | 8.8 | 9.0 | 8.6 | 8.9 | 4.0 |
| 53 | Oxyfluorfen | 16.59 | 14.1 | 12.8 | 13.6 | 12.4 | 11.1 | 12.8 | 9.0 |
| 54 | Parathion | 14.80 | 13.2 | 14.4 | 12.5 | 13.0 | 13.8 | 13.4 | 5.6 |
| 55 | Pirimiphos methyl | 14.24 | 9.6 | 9.8 | 9.5 | 9.5 | 9.5 | 9.6 | 1.3 |
| 56 | Propanil | 13.67 | 10.1 | 10.1 | 10.6 | 10.1 | 10.2 | 10.2 | 1.9 |
| 57 | Pyridaben | 20.87 | 10.7 | 12.8 | 13.1 | 11.5 | 11.1 | 11.8 | 8.9 |
| 58 | Quinoxyfen | 18.00 | 11.7 | 11.5 | 12.1 | 11.7 | 11.5 | 11.7 | 2.1 |
| 59 | Simazine | 12.29 | 9.3 | 10.4 | 9.5 | 10.2 | 10.2 | 9.9 | 4.9 |
| 60 | Tebuconazole | 18.38 | 10.2 | 10.6 | 10.5 | 11.1 | 10.3 | 10.5 | 3.0 |
| 61 | Triadimefon | 14.87 | 11.1 | 10.4 | 10.1 | 10.6 | 9.0 | 10.3 | 7.6 |
| 62 | Triazophos | 17.65 | 7.4 | 9.1 | 8.5 | 8.0 | 7.2 | 8.0 | 9.9 |
| 63 | Ametryn | 14.00 | 10.7 | 10.1 | 10.3 | 10.1 | 10.4 | 10.3 | 2.2 |
| 64 | Azaconazole | 16.83 | 13.8 | 13.6 | 14.5 | 13.7 | 13.3 | 13.8 | 3.2 |
| 65 | Bupirimate | 16.66 | 11.0 | 10.4 | 11.3 | 11.1 | 10.4 | 10.8 | 3.8 |
| 66 | Butachlor | 16.01 | 9.9 | 9.8 | 10.6 | 9.7 | 9.4 | 9.9 | 4.4 |
| 67 | Chlorthal dimethyl | 14.73 | 9.4 | 8.9 | 9.4 | 8.8 | 8.5 | 9.0 | 4.4 |
| 68 | Dicloran | 12.19 | 6.8 | 8.3 | 8.4 | 7.6 | 6.3 | 7.5 | 12.1 |
| 69 | Diethofencarb | 14.63 | 12.3 | 10.8 | 11.2 | 10.9 | 10.7 | 11.2 | 6.0 |
| 70 | Dimepiperate | 15.74 | 13.3 | 11.4 | 13.6 | 12.4 | 13.4 | 12.8 | 7.0 |
| 71 | Dimethenamid | 13.61 | 10.0 | 9.6 | 10.1 | 10.4 | 9.5 | 9.9 | 3.6 |
| 72 | Etoxazole | 19.03 | 11.0 | 11.1 | 11.1 | 10.9 | 11.2 | 11.0 | 0.9 |
| 73 | Fluacrypyrim | 17.38 | 11.1 | 10.8 | 11.0 | 11.2 | 10.6 | 11.0 | 2.3 |
| 74 | Lenacil | 18.14 | 10.6 | 12.3 | 11.4 | 11.6 | 10.6 | 11.3 | 6.6 |
| 75 | Pyriminobac methyl 1 | 17.96 | 12.8 | 12.3 | 12.5 | 12.7 | 12.6 | 12.6 | 1.5 |
| 76 | Pyriminobac methyl 2 | 12.88 | 10.8 | 10.9 | 11.0 | 10.4 | 10.8 | 10.8 | 2.1 |
| 77 | Pyroquilon | 19.53 | 10.3 | 9.2 | 9.7 | 9.7 | 10.0 | 9.8 | 4.2 |
| 78 | Tetradifon | 13.87 | 7.5 | 9.3 | 9.4 | 8.5 | 8.1 | 8.6 | 9.1 |
| 79 | Tolclofos-methyl | 16.61 | 9.2 | 9.2 | 9.2 | 9.2 | 9.1 | 9.2 | 0.6 |
| 80 | Uniconazole P | 13.66 | 11.5 | 12.4 | 10.8 | 11.5 | 10.6 | 11.4 | 6.3 |
| 81 | Acetochlor | 17.83 | 9.3 | 8.7 | 8.8 | 9.3 | 8.9 | 9.0 | 3.3 |
| 82 | Benalaxyl | 13.57 | 10.7 | 9.9 | 10.3 | 10.2 | 9.8 | 10.2 | 3.5 |
| 83 | Benfuresate | 11.71 | 9.6 | 9.3 | 9.4 | 9.7 | 9.6 | 9.5 | 1.6 |
| 84 | Cadusafos | 11.37 | 8.2 | 8.3 | 8.0 | 8.6 | 7.9 | 8.2 | 3.5 |
| 85 | Chlorpropham | 15.61 | 8.9 | 8.5 | 8.2 | 9.1 | 8.9 | 8.7 | 4.4 |
| 86 | Diclocymet 1 | 15.91 | 10.4 | 10.8 | 10.4 | 10.9 | 10.2 | 10.5 | 2.9 |
| 87 | Diclocymet 2 | 15.40 | 10.0 | 10.4 | 10.8 | 9.9 | 10.0 | 10.2 | 3.4 |
| 88 | Dimethametryn | 14.49 | 12.0 | 10.7 | 11.7 | 11.6 | 11.4 | 11.5 | 4.3 |
| 89 | Esprocarb | 21.83 | 9.3 | 9.4 | 9.3 | 9.7 | 9.1 | 9.4 | 2.5 |
| 90 | Etofenprox | 16.08 | 12.8 | 12.6 | 12.7 | 12.9 | 12.4 | 12.7 | 1.5 |
| 91 | Fenothiocarb | 13.27 | 10.4 | 10.3 | 10.4 | 10.7 | 11.0 | 10.6 | 2.9 |
| 92 | Iprobenfos | 16.92 | 9.6 | 9.0 | 10.0 | 10.0 | 9.2 | 9.6 | 4.7 |
| 93 | Isoxathion | 17.61 | 6.6 | 8.0 | 8.0 | 6.7 | 6.9 | 7.3 | 9.8 |
| 94 | Mepronil | 14.04 | 11.4 | 11.1 | 11.8 | 11.6 | 11.5 | 11.5 | 2.2 |
| 95 | Prometryn | 10.85 | 10.2 | 9.7 | 10.0 | 10.9 | 9.8 | 10.1 | 4.8 |
| 96 | Propachlor | 16.41 | 9.4 | 7.6 | 7.0 | 8.0 | 7.5 | 7.9 | 11.5 |
| 97 | Prothiofos | 15.99 | 8.7 | 9.7 | 8.9 | 9.3 | 9.2 | 9.1 | 4.4 |
| 98 | Pyrifenox 1 | 12.89 | 10.2 | 10.0 | 10.6 | 10.5 | 10.6 | 10.4 | 2.3 |
| 99 | Pyrimethanil | 13.94 | 9.4 | 9.4 | 9.6 | 10.5 | 8.9 | 9.6 | 6.0 |
| 100 | Simetryn | 13.06 | 11.0 | 10.6 | 9.4 | 10.2 | 10.7 | 10.4 | 6.0 |
| 101 | Terbacil | 14.82 | 8.7 | 10.0 | 9.9 | 10.2 | 9.2 | 9.6 | 6.6 |
| 102 | Tetraconazole | 18.31 | 11.9 | 11.6 | 11.7 | 10.9 | 13.4 | 11.9 | 7.7 |
| 103 | Thenylchlor | 16.58 | 7.1 | 8.1 | 8.8 | 8.0 | 7.8 | 8.0 | 7.3 |
| 104 | Tribufos | 16.66 | 9.0 | 10.4 | 9.7 | 9.8 | 8.3 | 9.4 | 8.4 |
| 105 | Tricyclazole | 15.72 | 4.4 | 6.9 | 6.3 | 5.4 | 4.7 | 5.5 | 18.8 |
| 106 | Zoxamide (decomposed) | 13.40 | 10.5 | 11.1 | 11.0 | 10.3 | 9.6 | 10.5 | 5.7 |
| 107 | Benoxacor | 14.44 | 4.2 | 4.7 | 5.0 | 4.5 | 3.8 | 4.4 | 10.1 |
| 108 | Bromacil | 13.70 | 6.6 | 8.1 | 8.1 | 8.4 | 7.9 | 7.8 | 9.0 |
| 109 | Bromobutide | 16.17 | 11.7 | 9.7 | 10.5 | 11.8 | 10.2 | 10.8 | 8.7 |
| 110 | Butamifos | 13.56 | 10.3 | 12.0 | 11.7 | 11.0 | 10.9 | 11.2 | 6.3 |
| 111 | Dichlofenthion | 15.12 | 9.7 | 9.3 | 9.5 | 10.2 | 9.1 | 9.6 | 4.6 |
| 112 | Diphenamid | 16.42 | 12.2 | 11.5 | 12.2 | 11.9 | 12.1 | 12.0 | 2.3 |
| 113 | Hexaconazole | 14.00 | 10.0 | 11.6 | 11.4 | 9.9 | 11.4 | 10.9 | 7.7 |
| 114 | Mefenoxam | 16.33 | 16.3 | 15.5 | 17.4 | 16.6 | 16.1 | 16.4 | 4.4 |
| 115 | Napropamide | 17.40 | 10.6 | 10.6 | 10.8 | 10.5 | 10.1 | 10.5 | 2.5 |
| 116 | Oxadixyl | 16.07 | 9.2 | 10.9 | 10.2 | 9.6 | 9.1 | 9.8 | 7.5 |
| 117 | Paclobutrazol | 19.31 | 11.8 | 12.0 | 12.8 | 12.3 | 12.1 | 12.2 | 3.1 |
| 118 | Phenothrin 1 | 19.42 | 13.8 | 10.0 | 11.1 | 12.0 | 10.5 | 11.5 | 13.3 |
| 119 | Phenothrin 2 | 18.98 | 11.5 | 11.2 | 11.0 | 11.0 | 11.2 | 11.2 | 1.8 |
| 120 | Piperophos | 12.94 | 9.9 | 10.0 | 11.3 | 10.9 | 10.5 | 10.5 | 5.5 |
| 121 | Prohydrojasmon 1 | 13.23 | 8.8 | 8.5 | 8.4 | 8.9 | 8.1 | 8.5 | 3.8 |
| 122 | Prohydrojasmon 2 | 12.42 | 11.8 | 12.2 | 11.2 | 14.5 | 12.2 | 12.4 | 10.3 |
| 123 | Propazine | 18.63 | 9.7 | 8.5 | 9.3 | 9.8 | 8.8 | 9.2 | 6.0 |
| 124 | Pyributicarb | 15.51 | 13.0 | 12.7 | 13.0 | 13.1 | 12.9 | 12.9 | 1.1 |
| 125 | Pyrifenox 2 | 15.63 | 10.6 | 9.9 | 11.1 | 10.0 | 9.7 | 10.3 | 5.5 |
| 126 | Quinalphos | 19.16 | 10.1 | 11.1 | 11.8 | 11.6 | 10.1 | 11.0 | 7.3 |
| 127 | Tebufenpyrad | 24.05 | 11.1 | 10.7 | 11.4 | 10.8 | 10.9 | 11.0 | 2.7 |
| 128 | Tolfenpyrad | 14.78 | 11.5 | 11.5 | 11.7 | 11.5 | 11.4 | 11.5 | 0.9 |
| 129 | Aldrin | 16.26 | 7.4 | 8.5 | 9.7 | 8.5 | 9.2 | 8.7 | 10.0 |
| 130 | cis-Chlordane | 14.97 | 8.5 | 9.4 | 9.6 | 8.5 | 9.3 | 9.1 | 5.7 |
| 131 | Dicofol | 16.78 | 11.7 | 10.7 | 10.6 | 10.9 | 10.8 | 11.0 | 3.8 |
| 132 | Dieldrin | 17.19 | 8.2 | 8.3 | 10.4 | 7.4 | 10.0 | 8.8 | 14.4 |
| 133 | Endrin | 14.07 | 8.7 | 10.0 | 10.7 | 10.6 | 8.5 | 9.7 | 10.7 |
| 134 | Heptachlor | 16.02 | 5.9 | 6.8 | 6.6 | 6.8 | 6.0 | 6.4 | 6.7 |
| 135 | trans-Chlordane | 14.40 | 9.9 | 9.0 | 9.7 | 9.7 | 9.3 | 9.5 | 3.8 |
| 136 | 1-Naphthylacetamide | 15.87 | 14.4 | 13.2 | 14.3 | 13.6 | 14.1 | 13.9 | 3.6 |
| 137 | Bromophos ethyl | 16.80 | 8.9 | 8.6 | 9.5 | 8.8 | 8.6 | 8.9 | 4.1 |
| 138 | Carboxin | 15.98 | 3.5 | 3.6 | 3.4 | 3.7 | 3.5 | 3.5 | 3.4 |
| 139 | Chlorbenside | 16.42 | 10.0 | 9.7 | 9.5 | 10.0 | 9.8 | 9.8 | 1.9 |
| 140 | Chlorofenson | 24.99 | 6.8 | 8.6 | 8.7 | 8.2 | 7.4 | 7.9 | 10.6 |
| 141 | clomazone | 12.47 | 8.0 | 8.3 | 8.9 | 8.9 | 7.9 | 8.4 | 5.7 |
| 142 | Disulfoton | 12.98 | 7.5 | 7.4 | 7.3 | 8.1 | 7.3 | 7.5 | 4.6 |
| 143 | Epoxiconazole | 18.61 | 11.4 | 11.3 | 11.8 | 11.1 | 11.3 | 11.4 | 2.1 |
| 144 | Ethofumesate | 14.37 | 10.2 | 10.0 | 10.2 | 10.5 | 9.3 | 10.0 | 4.6 |
| 145 | Fenamidone | 19.17 | 11.8 | 11.1 | 10.9 | 12.1 | 11.1 | 11.4 | 4.7 |
| 146 | Flutriafol | 16.28 | 12.6 | 11.3 | 11.7 | 11.2 | 11.5 | 11.6 | 4.7 |
| 147 | Isazophos | 12.96 | 10.1 | 9.4 | 9.6 | 10.4 | 9.4 | 9.8 | 4.6 |
| 148 | Phorate | 11.79 | 8.3 | 8.5 | 7.5 | 8.3 | 8.4 | 8.2 | 4.9 |
| 149 | Picolinafen | 18.97 | 12.9 | 11.5 | 11.8 | 11.2 | 12.6 | 12.0 | 6.1 |
| 150 | Propaphos | 15.89 | 10.8 | 11.2 | 11.7 | 10.7 | 10.9 | 11.1 | 3.5 |
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