Table 1. List of analysed pesticides (alphabetical order), their chemical class, agricultural role and method validation results for both LC-MSMS and GC-ECD.
| Beeswax | Honeybees | Honey | LOD μg/kg | LOQ μg/kg | |||||||
|---|---|---|---|---|---|---|---|---|---|---|---|
| No. | Pesticide | Chemical Class | Role | %recovery | %RSD | %recovery | %RSD | %recovery | %RSD | ||
| 1 | Acetamiprid | neonicotinoid | I | 47.2 | 5.4 | 119.8 | 11.1 | 56.3 | 2.4 | 0.003 | 0.010 |
| 2 | Azoxystrobin | strobilurin | F | 85.5 | 8.8 | 136.3 | 8.7 | 58.0 | 13.0 | 0.003 | 0.010 |
| 3 | Deltamethrin | pyrethroid | I | 94.1 | 5.8 | x | x | x | x | 0.116 | 0.387 |
| 4 | Boscalid | anilide | F | 61.0 | 6.1 | 118.1 | 7.0 | 73.3 | 11.5 | 0.015 | 0.050 |
| 5 | Carbendazim | carbamate | F | 50.8 | 3.7 | 67.7 | 10.5 | 38.8 | 6.8 | 0.003 | 0.010 |
| 6 | Carbofuran | carbamate | I | 59.9 | 4.0 | 102.4 | 4.6 | 55.9 | 7.3 | 0.015 | 0.050 |
| 7 | Chlorpyrifos | organophosphate | I | 81.7 | 4.6 | 54.4 | 5.1 | 60.3 | 15.7 | 0.015 | 0.050 |
| 8 | Clofentezine | tetrazine | I | 63.8 | 3.6 | 80.1 | 6.9 | 78.3 | 16.6 | 0.030 | 0.100 |
| 9 | Cyflufenamid | amide | F | 48.2 | 2.5 | 61.3 | 7.9 | 68.0 | 15.7 | 0.015 | 0.050 |
| 10 | Cypermethrin | pyrethroid | I | 112.3 | 7.1 | x | x | x | x | 0.588 | 1.959 |
| 11 | Cyprodinil | anilinopyrimidine | F | 59.8 | 6.2 | 52.20 | 5.9 | 56.1 | 6.1 | 0.003 | 0.010 |
| 12 | Difenoconazole | azole | F | 94.7 | 3.3 | 62.3 | 10.2 | 77.6 | 14.0 | 0.003 | 0.010 |
| 13 | Dimethoate | organophosphate | I | 39.6 | 7.1 | 92.2 | 10.5 | 46.8 | 12.6 | 0.030 | 0.100 |
| 14 | Endosulfan | organochlorine | I | 82.2 | 9.7 | x | x | x | x | 0.055 | 0.184 |
| 15 | Fenitrothion | organophosphate | I | 61.3 | 6.4 | 366.9 | 66.0 | 80.7 | 17.4 | 0.150 | 0.500 |
| 16 | Fenoxycarb | carbamate | I | 71.9 | 2.5 | 89.6 | 9.4 | 67.8 | 12.6 | 0.003 | 0.010 |
| 17 | Imidacloprid | neonicotinoid | I | 55.2 | 15.9 | 111.2 | 19.3 | 50.9 | 8.2 | 0.030 | 0.100 |
| 18 | Iprodione | dicarboximide | F | 50.0 | 2.9 | 94.9 | 12.6 | 72.6 | 5.5 | 0.150 | 0.500 |
| 19 | Malathion | organophosphorus | I | 94.3 | 6.6 | 154.9 | 14.0 | 84.3 | 21.3 | 0.030 | 0.100 |
| 20 | Metalaxyl | xylalanine | F | 79.3 | 1.5 | 101.0 | 5.5 | 74.0 | 9.8 | 0.015 | 0.050 |
| 21 | Methomyl | carbamate | I | 110.0 | 5.6 | 111.5 | 13.3 | 133.1 | 4.5 | 0.018 | 0.059 |
| 22 | O,P' -DDT | organochlorine | I | 62.5 | 4.4 | x | x | x | x | 0.118 | 0.629 |
| 23 | P,P' -DDD | organochlorine | I | 74.4 | 4.4 | x | x | x | x | 0.056 | 0.187 |
| 24 | P,P' -DDE | organochlorine | I | 57.1 | 7.3 | x | x | x | x | 0.056 | 0.187 |
| 25 | P,P' DDT | organochlorine | I | 63.6 | 4.3 | x | x | x | x | 0.056 | 0.186 |
| 26 | Penconazole | azole | F | 82.1 | 7.9 | 99.7 | 4.0 | 73.6 | 12.3 | 0.003 | 0.010 |
| 27 | Permethrin | pyrethroid | I | 112.7 | 7.0 | x | x | x | x | 0.554 | 1.847 |
| 28 | Piperonyl-butoxide | unclassified | I | 61.7 | 4.5 | 96.5 | 4.5 | 83.0 | 22.4 | 0.030 | 0.100 |
| 29 | Pirimicarb | carbamate | I | 56.1 | 25.2 | 104.7 | 6.3 | 56.3 | 4.8 | 0.003 | 0.010 |
| 30 | Profenofos | organophosphorus | I | 56.6 | 3.3 | 70.2 | 8.9 | 70.6 | 13.4 | 0.003 | 0.010 |
| 31 | Pyraclostrobin | strobilurin | F | 67.2 | 3.1 | 93.0 | 3.4 | 72.7 | 17.9 | 0.015 | 0.050 |
| 32 | Tebuconazole | azole | F | 79.6 | 2.9 | 114.2 | 23.4 | 75.2 | 12.5 | 0.003 | 0.010 |
| 33 | Tebufenozide | diacylhydrazine | I | 72.1 | 13.9 | 118.1 | 24.8 | 90.3 | 12.4 | 0.030 | 0.100 |
| 34 | Thiram | dimethyldithiocarbamate | F | 60.3 | 7.9 | 53.6 | 0.7 | 98.5 | 29.8 | 0.030 | 0.100 |
| 35 | Thiamethoxam | neonicotinoid | I | 73.8 | 6.8 | 109.5 | 16.4 | 98.1 | 17.4 | 0.150 | 0.500 |
| 36 | Trifloxystrobin | strobilurin | F | 54.8 | 1.7 | 66.7 | 7.3 | 77.1 | 17.2 | 0.003 | 0.010 |
Symbol interpretation; x = hive product was not analysed; F = Fungicide and I = Insecticide