bozena lozowicka*, ewa rutkowska, izabela hrynko ... · supplement: determination of pesticides in...

Open Chem., 2015; 13: S40–S51

Research Article Open Access

Bozena Lozowicka*, Ewa Rutkowska, Izabela Hrynko

Supplement: Simultaneous determination of 223 pesticides in tobacco by GC with simultaneous electron capture and nitrogen-phosphorous detection and mass spectrometric confirmation

*Corresponding author: Bozena Lozowicka: Plant Protection Institute - National Research Institute, Regional Experimental Station, Laboratory of Pesticide Residues, Chelmonskiego 22, Postal code: 15-195 Bialystok, Poland, E-mail: B.Lozowicka@iorpib.poznan.pl Ewa Rutkowska, Izabela Hrynko: Plant Protection Institute - National Research Institute, Regional Experimental Station, Laboratory of Pesticide Residues, Chelmonskiego 22, Postal code: 15-195 Bialystok, Poland

Suppementary Table 1: Validation parameters and matrix effect of LSE method in tobacco studied by GC-µECD/NPD. Negative values of matrix effects mean suppression of the signal and positives values enhancement.

Active substance (Pesticide type)

Substance group EC NP Spiking level (mg/kg)

Mean recovery ± RSD(%)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

1. Napropamide (H) Alkanamide + 0.05 97 ± 4 1 0.01 0.003

2. Cyflufenamid (F) Amide + 0.01 78 ± 9 30 0.01 0.003

3. Amitraz (I) Amidine + 0.01 n.d. -32 0.01 0.003

4. Cyprodinil (F) Anilinopyrimidine + 0.01 82 ± 7 11 0.009 0.003

5. Mepanipirym (F) + 0.01 65 ± 5 7 0.01 0.003

6. Pyrimethanil (F) + 0.01 85 ± 10 5 0.01 0.003

7. Chlorantraniliprole1 (I) Anthranilic diamide ++ + 0.01 86 ± 15 -98 0.01 0.003

8. Fenoxaprop-p-ethyl (H) Aryloxyphenoxypropionate + ++ 0.05 92 ± 3 38 0.03 0.009

9. Fluazifop-p-butyl1 (H) + 0.01 87 ± 6 42 0.03 0.009

10. Propaquizafop (H) ++ + 0.05 69 ± 13 -71 0.03 0.009

11. Quizalofop-p-ethyl (H) ++ + 0.01 68 ± 6 2 0.01 0.003

12. Fluopicolide (F) Benzamide + 0.01 83 ± 13 13 0.01 0.003

13. Propyzamide (H) ++ + 0.01 97 ± 7 36 0.01 0.003

14. Bromopropylate (A) Benzilate + 0.01 96 ± 13 65 0.01 0.003

15. Fuberidazole (F) Benzimidazole + 0.01 n.d. 1 - -

16. Thiabendazole (I) + 0.01 n.d. 23 - -

17. Dichlobenil (H) Benzonitrile ++ + 0.01 45 ± 5 8 0.01 0.003

18. Metrafenone (F) Benzophenone + 0.01 44 ± 4 16 0.01 0.003

Supplement: Determination of pesticides in tobacco and nitrogen-phosphorous detection by MS S41

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

19. Teflubenzuron (I) Benzoylurea + 0.05 69 ± 9 171 0.02 0.006

20. Tetradifon (I) Bridged diphenyl + 0.01 83 ± 5 8 0.01 0.003

21. Carbaryl1 (I) Carbamate + 0.01 102 ± 7 248 0.02 0.006

22. Carbofuran1 (I) + 0.01 75 ± 5 207 0.02 0.006

23. Carbosulfan (I) + 0.01 n.d. -60 - -

24. Chlorpropham (H) + 0.05 84 ± 10 -52 0.01 0.003

25. Fenoxycarb (I) + 0.01 58 ± 9 105 0.01 0.003

26. Iprowalikarb (F) + 0.05 84 ± 6 80 0.01 0.003

27. Isoprocarb (I) + 0.01 69 ± 6 -77 0.01 0.003

28. Pirimicarb1.2 (I) + 0.01 78 ± 3 -1 0.01 0.003

29. Pirimicarb desmethyl (I) + 0.01 80 ± 7 8 0.01 0.003

30. Propham (H) + 0.05 77 ± 7 16 0.02 0.006

31. Propoxur1 (I) + 0.01 91 ± 10 -8 0.02 0.006

32. Boscalid (F) Carboxamide ++ + 0.01 72 ± 6 0.3 0.01 0.003

33. Diflufenican (DFF) (H) + 0.01 89 ± 10 75 0.01 0.003

34. Hexythiazox (A) ++ + 0.05 89 ± 8 -50 0.04 0.012

35. Acetochlor (H) Chloroacetamide ++ + 0.01 80 ± 10 1 0.01 0.003

36. Dimethenamid (H) ++ + 0.05 80 ± 11 87 0.02 0.006

37. Metazachlor (H) ++ + 0.01 97 ± 15 11 0.01 0.003

38. Metolachlor (H) ++ + 0.05 79 ± 6 5 0.02 0.006

39. Propachlor (H) ++ + 0.05 82 ± 10 21 0.02 0.006

40. Chlorothalonil1 (F) Chlorine-substituted aromatics

+ 0.01 91 ± 11 70 0.01 0.003

41. Dicloran1 (F) + 0.01 77 ± 3 -0.2 0.01 0.003

42. HCB (Hexachlorobenzene)1 (F)

+ 0.01 69 ± 3 -10 0.005 0.001

43. Quintozene (PCNB) (F) + 0.01 99 ± 6 3 0.01 0.003

44. Tecnazene (TCNB) (F) + 0.01 67 ± 6 4 0.009 0.003

45. Tolclofos methyl (F) + ++ 0.01 84 ± 5 21 0.01 0.003

46. Cymoxanil1 (F) Cyanoacetamide oxime + 0.05 49 ± 7 33 0.04 0.012

47. Iprodione1 (F) Dicarboximide + 0.05 92 ± 7 1870 0.02 0.006

48. Procymidone (F) ++ + 0.01 85 ± 8 12 0.01 0.003

49. Pendimethalin1 (H) Dinitroaniline ++ + 0.01 89 ± 14 8 0.01 0.003

50. Trifluralin1 (H) ++ + 0.01 97 ± 6 2 0.01 0.003

51. Nitrofen1 (H) Diphenyl ether + 0.01 78 ± 8 -17 0.009 0.003

52. Oxyflurofen (H) + 0.01 89 ± 8 22 0.009 0.003

53. Fenhexamid (F) Hydroxyanilide + 0.05 78 ± 12 -103 0.02 0.006

54. Fenamidon (F) Imidazole ++ + 0.01 103 ± 8 7 0.01 0.003

55. Imazalil (F) ++ + 0.01 41 ± 10 72 0.02 0.006

56. Prochloraz (F) ++ + 0.01 88 ± 9 -40 0.01 0.003

57. Triflumizole (F) ++ + 0.01 85 ± 11 27 0.02 0.006

58. Isoxaflutole (H) Isoxazole ++ + 0.05 74 ± 5 61 0.02 0.006

ContinuedSuppementary Table 1: Validation parameters and matrix effect of LSE method in tobacco studied by GC-µECD/NPD. Negative values of matrix effects mean suppression of the signal and positives values enhancement.

S42 Bozena Lozowicka, Ewa Rutkowska, Izabela Hrynko

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

59. Clomazone1.2 (H) Isoxazolidinone + 0.01 88 ± 10 5 0.01 0.003

60. Dimethomorph1 (F) Morpholine + 0.05 86 ± 3 -87 0.03 0.009

61. Fenpropimorph (F) + 0.05 43 ± 7 5 0.02 0.006

62. Acetamiprid1 (I) Neonicotinoid + 0.01 124 ± 4 20 0.01 0.003

63. Thiacloprid (I) ++ + 0.01 n.d. 16 - -

64. Thiametoxam1 (I) ++ + 0.01 52 ± 14 16 0.02 0.006

65. Aldrine1 (I) Organochlorine + 0.01 77 ± 12 -17 0.005 0.001

66. Alpha endosulfan1 (I) + 0.01 76 ± 3 -91 0.008 0.002

67. Alpha HCH1 (I) + 0.01 72 ± 8 -13 0.005 0.001

68. Beta endosulfan1 (I) + 0.01 84 ± 5 -2 0.008 0.002

69. Beta HCH1 (I) + 0.01 75 ± 4 -30 0.005 0.001

70. Dicofol (A) + 0.01 75 ± 4 9 0.01 0.003

71. Dieldrin1 (I) + 0.01 100 ± 7 -24 0.005 0.001

72. Sulfate endosulfan1 (I) Organochlorine + 0.01 78 ± 6 29 0.008 0.002

73. Endrin1 (I) + 0.01 94 ± 3 3364 0.005 0.001

74. Heptachlor1 (I) + 0.01 69 ± 7 -20 0.005 0.001

75. Heptachlor epoxide1 (I) + 0.01 77 ± 5 -27 0.005 0.001

76. Methoxychlor (DMDT)1 (I) + 0.01 92 ± 8 2162 0.01 0.003

77. o.p’-DDT1 (I) + 0.01 89 ± 6 -19 0.005 0.001

78. p.p’-DDD1 (I) + 0.01 85 ± 11 -19 0.005 0.001

79. p.p’-DDE1 (I) + 0.01 97 ± 5 -29 0.005 0.001

80. p.p’-DDT1 (I) + 0.01 97 ± 2 3186 0.005 0.001

81. Azinphos ethyl1 (I) Organophosphate + ++ 0.01 84 ± 6 3 0.01 0.003

82. Azinphos methyl1 (I) + ++ 0.01 95 ± 4 54 0.01 0.003

83. Chlorfenvinphos1 (I) + ++ 0.01 83 ± 7 0.1 0.008 0.002

84. Bromofos ethyl1 (I) + ++ 0.01 76 ± 4 5 0.009 0.003

85. Bromofos methyl (I) + ++ 0.01 76 ± 3 2 0.009 0.003

86. Cadusafos (I) + 0.01 67 ± 3 28 0.008 0.002

87. Chlorpyrifos1 (I) ++ + 0.01 81 ± 5 8 0.006 0.002

88. Chlorpyrifos methyl1 (I) ++ + 0.01 81 ± 8 8 0.006 0.002

89. Coumphos (I) + ++ 0.05 84 ± 6 86 0.03 0.009

90. Diazinon1 (I) + 0.01 83 ± 3 45 0.01 0.003

91. Dichlorvos1 (I) ++ + 0.01 76 ± 16 61 0.01 0.003

92. Dicrotophos (I) + 0.01 48 ± 5 211 0.01 0.003

93. Dimethoate1 (I) + ++ 0.01 88 ± 3 38 0.01 0.003

94. EPN (I) + ++ 0.01 73 ± 8 5 0.009 0.003

95. Ethion (I) + ++ 0.01 96 ± 7 59 0.01 0.003

96. Ethoprophos1 (I) + 0.01 83 ± 4 32 0.01 0.003

97. Fenchlorfos1 (I) + ++ 0.01 81 ± 9 3 0.01 0.003

98. Fenitrothion1 (I) + ++ 0.01 77 ± 6 5 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

99. Fention1 (I) Organophosphate + 0.01 68 ± 8 21 0.01 0.003

100. Formothion1 (I) ++ + 0.01 88 ± 3 3 0.01 0.003

101. Fostiazate (I) + 0.01 63 ± 8 77 0.01 0.003

102. Heptenophos (I) Organophosphate + 0.01 85 ± 4 55 0.01 0.003

103. Isocarbophos (A) + 0.01 68 ± 9 89 0.01 0.003

104. Isofenphos (I) + 0.01 89 ± 10 57 0.01 0.003

105. Isofenfos methyl (I) + 0.01 86 ± 9 35 0.01 0.003

106. Malaoxon (I) + 0.01 84 ± 14 37 0.01 0.003

107. Malathion1 (I) + 0.01 93 ± 13 66 0.01 0.003

108. Mecarbam (I) ++ + 0.01 92 ± 8 10 0.01 0.003

109. Methacrifos (F) + ++ 0.01 67 ± 4 28 0.01 0.003

110. Methidathion1 (I) + ++ 0.01 85 ± 3 7 0.01 0.003

111. Mevinphos (I) + 0.01 80 ± 14 33 0.01 0.003

112. Paraoxon ethyl (I) + ++ 0.01 72 ± 11 -4 0.01 0.003

113. Paraoxon methyl (I) + ++ 0.01 72 ± 12 67 0.01 0.003

114. Parathion ethyl1 (I) + ++ 0.01 81 ± 4 6 0.01 0.003

115. Parathion methyl1 (I) + ++ 0.01 81 ± 5 2 0.01 0.003

116. Phentoate (I) + ++ 0.01 78 ± 9 2 0.01 0.003

117. Phorate1 (I) + 0.01 67 ± 10 46 0.01 0.003

118. Phosalone1 (I) + ++ 0.01 88 ± 6 16 0.01 0.003

119. Phosmet (I) + ++ 0.01 93 ± 4 98 0.01 0.003

120. Pirimiphos ethyl (I) + 0.01 83 ± 4 47 0.009 0.003

121. Pirimiphos methyl1 (I) + 0.01 86 ± 15 46 0.009 0.003

122. Profenofos1 (I) + ++ 0.01 91 ± 5 42 0.01 0.003

123. Quinalphos (I) + ++ 0.01 90 ± 10 31 0.008 0.002

124. Tetrachlorwinfos1 (I) ++ + 0.01 93 ± 7 94 0.01 0.003

125. Triazophos (I) + 0.01 94 ± 7 52 0.01 0.003

126. Indoxacarb1 (I) Oxadiazine + 0.01 82 ± 4 -79 0.01 0.003

127. Flutolanil (F) Oxathin ++ + 0.05 108 ± 9 154 0.03 0.009

128. Famoksadone1 (F) Oxazole ++ + 0.05 53 ± 5 79 0.01 0.003

129. Vinclozolin (F) + 0.01 86 ± 6 9 0.01 0.003

130. Chlozolinate (F) Oxazolidin + 0.01 74 ± 4 -7 0.01 0.003

131. Flufenacet (H) Oxyacetamide + 0.01 78 ± 9 1 0.01 0.003

132. Benalaxyl1 (F) Phenylamide + 0.01 83 ± 13 26 0.01 0.003

133. Metalaxyl1.2 (F) + 0.01 84 ± 5 127 0.01 0.003

134. Oksadixyl1 (F) + 0.01 68 ± 8 14 0.01 0.003

135. Fipronil (I) Phenylpyrazole + 0.01 93 ± 14 184 0.009 0.003

136. Fluazinam (F) Phenylpyridinamine + 0.01 107 ± 5 -21 0.01 0.003

137. Fludioxonil (F) Phenylpyrole + 0.01 76 ± 4 -24 0.01 0.003

138. Pencycuron (F) Phenylurea + 0.05 54 ± 5 -76 0.02 0.006

139. Isoprothiolane (F) Phosphorothiolate + 0.01 89 ± 7 51 0.01 0.003

140. Pyrazofos (I) + ++ 0.01 92 ± 10 38 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

141. Captafol (F) Phthalimide + 0.01 107 ± 8 928 0.01 0.003

142. Captan1 (F) + 0.01 84 ± 4 1535 0.01 0.003

143. Folpet1 (F) + 0.01 43 ± 3 71 0.01 0.003

144. Tebufenpyrad (A) Pyrazole + 0.01 70 ± 14 -42 0.01 0.003

145. Acrinathrin (I) Pyrethroid + 0.01 100 ± 7 454 0.01 0.003

146. Bifenthrin1 (I) + 0.01 86 ± 4 27 0.01 0.003

147. Cyfluthrin1 (I) + 0.05 86 ± 8 36 0.02 0.006

148. Cypermethrin1.2 (I) + 0.05 79 ± 11 -69 0.01 0.003

149. Deltamethrin1 (I) + 0.05 97 ± 5 4 0.01 0.003

150. Esfenvalerate1 (I) + 0.01 76 ± 5 55 0.01 0.003

151. Fenpropathrin (I) + 0.01 84 ± 7 13 0.01 0.003

152. Fenvalerate1 (I) + 0.01 70 ± 3 -75 0.01 0.003

153. Gamma HCH (Lindane)1 (I) + 0.01 85 ± 11 -9 0.005 0.002

154. Lambda cyhalothrin1 (I) + 0.01 83 ± 5 10 0.01 0.003

155. Permethrin1 (I) + 0.05 99 ± 4 18 0.04 0.012

156. Pyrethrin1 (I) + 0.05 105 ± 4 35 0.04 0.012

157. Tau-Fluvalinate (I) + 0.01 75 ± 17 458 0.01 0.003

158. Tefluthrin1 (I) + 0.01 70 ± 1 21 0.009 0.003

159. Tetramethrin (I) + 0.05 101 ± 5 326 0.03 0.009

160. Zoxamide (F) + 0.01 84 ± 3 -79 0.009 0.003

161. Chloridazon (H) Pyridazinone ++ + 0.01 88 ± 4 -20 0.009 0.003

162. Flurtamone (H) + ++ 0.01 84 ± 5 -15 0.01 0.003

163. Pyridaben (A) ++ + 0.05 86 ± 10 28 0.02 0.006

164. Flonicamid (I) Pyridine ++ + 0.01 n.d. -1 - -

165. Fenarimol (F) Pyrimidine ++ + 0.01 78 ± 7 4 0.01 0.003

166. Bupirimate (F) Pyrimidinol ++ + 0.01 90 ± 4 6 0.01 0.003

167. Quinoxyfen (F) Quinoline ++ + 0.01 106 ± 4 61 0.009 0.003

168. Azoxystrobin (F) Strobilurin ++ + 0.01 69 ± 7 -76 0.01 0.003

169. Dimoksystrobina (F) ++ + 0.01 85 ± 5 44 0.01 0.003

170. Fluoxastrobin (F) ++ + 0.01 69 ± 14 229 0.01 0.003

171. Kresoxim methyl (F) ++ + 0.01 80 ± 9 14 0.01 0.003

172. Picoxystrobin (F) ++ + 0.05 76 ± 7 -3 0.04 0.012

173. Pyraklostrobina (F) ++ + 0.05 113 ± 4 46 0.05 0.015

174. Trifloxystrobin (F) ++ + 0.01 91 ± 5 21 0.01 0.003

175. Propargite (A) Sulfite ester + 0.05 55 ± 19 325 0.05 0.015

176. Tritosulfuron (H) Sulfonylurea + 0.01 42 ± 15 95 0.01 0.003

177. Dichlofluanid (F) Sulphamide ++ + 0.01 63 ± 1 8 0.01 0.003

178. Tolylfluanid (F) ++ + 0.01 64 ± 3 21 0.01 0.003

179. Spirodiclofen (A) Tetronic acid + 0.01 83 ± 6 -44 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

180. Atrazine (H) Triazine + 0.01 67 ± 11 15 0.01 0.003

181. Cyanazine (H) + ++ 0.01 n.d. 21 - -

182. Cyprazine (H) + 0.01 57 ± 6 14 0.01 0.003

183. Procyazine (H) + ++ 0.01 60 ± 5 -51 0.01 0.003

184. Prometrine (H) + 0.01 75 ± 12 4 0.01 0.003

185. Propazine (H) + 0.01 62 ± 4 9 0.01 0.003

186. Simazine (H) + 0.01 71 ± 5 5 0.01 0.003

187. Terbuthylazine (H) + 0.01 75 ± 8 6 0.009 0.003

188. Terbutryn (H) + 0.01 56 ± 8 3 0.009 0.003

189. Metamitron (H) Triazinone + 0.01 108 ± 6 27 0.01 0.003

190. Metribuzin (H) ++ + 0.01 81 ± 7 3 0.009 0.003

191. Azaconazole (F) Triazole ++ + 0.01 83 ± 7 41 0.01 0.003

192. Bitertanol (F) + 0.05 67 ± 4 8 0.02 0.006

193. Bromuconazole (F) ++ + 0.01 95 ± 6 62 0.01 0.003

194. Cyproconazole (F) + 0.01 59 ± 5 -33 0.01 0.003

195. Difenoconazole (F) ++ + 0.05 59 ± 3 -19 0.01 0.003

196. Dinikonazol (F) ++ + 0.01 81 ± 8 32 0.009 0.003

197. Epoxiconazole (F) ++ + 0.01 92 ± 7 29 0.009 0.003

198. Etaconazole (F) ++ + 0.01 90 ± 9 -15 0.01 0.003

199. Fenbuconazole (F) + 0.01 70 ± 3 -10 0.01 0.003

200. Fluquinconazole (F) ++ + 0.01 79 ± 15 1 0.01 0.003

201. Flusilazole (F) + 0.01 92 ± 11 24 0.009 0.003

202. Flutriafol (F) + 0.05 85 ± 4 23 0.02 0.006

203. Hexaconazole (F) ++ + 0.01 105 ± 5 24 0.009 0.003

204. Imibenkonazol (F) + 0.01 69 ± 3 -28 0.01 0.003

205. Metkonazol (F) + 0.05 89 ± 10 29 0.02 0.006

206. Myclobutanyl (F) ++ + 0.01 82 ± 5 13 0.01 0.003

207. Paclobutrazol (F) + 0.01 70 ± 8 -42 0.01 0.003

208. Penconazole1 (F) ++ + 0.01 92 ± 14 15 0.009 0.003

209. Propiconazole (F) ++ + 0.01 90 ± 6 14 0.01 0.003

210. Prothioconazole (F) ++ + 0.01 61 ± 17 11 0.01 0.003

211. Tebuconazole (F) + 0.01 86 ± 7 2 0.01 0.003

212. Tetraconazole (F) ++ + 0.01 74 ± 6 10 0.01 0.003

213. Triadimefon (F) ++ + 0.01 90 ± 8 6 0.01 0.003

214. Triadimenol (F) + 0.05 77 ± 4 8 0.03 0.009

215. Triticonazole (F) ++ + 0.01 54 ± 3 -3 0.01 0.003

216. Buprofezin (I) Unclassified + 0.01 100 ± 5 22 0.01 0.003

217. DEET N.N-dietylo-m-toluamid (I)

+ 0.05 54 ± 3 197 0.03 0.009

218. Difenyloamina (F) + 0.01 81 ± 5 -9 0.01 0.003

219. Fenazaquin (I) + 0.01 90 ± 9 9 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

220. Flurochloridone (H) Unclassified + 0.01 84 ± 8 11 0.009 0.003

221. Pyriproxyfen (I) + 0.05 78 ± 11 29 0.02 0.006

222. Quinoclamine (H) + 0.01 81 ± 2 72 0.01 0.003

223. Lenacil (H) Uracil + 0.05 75 ± 4 2819 0.02 0.006

*LOQ - Limit of quantification**LOD - Limit of detection1 List of the pesticides employed for tobacco (CORESTA)2 Pesticides recommended for tobacco cultivation++ Preferred GC detectorn.d. not detected

Supplementary Table 2: Validation parameters and matrix effect of MSPD and QuEChERS methods in tobacco studied by GC-µECD/NPD. Negative values of matrix effects mean suppression of the signal and positives values enhancement.

Spiking level (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

MSPD QuEChERS

1. Napropamide (H) 0.05 85 ± 11 12 0.01 0.003 88 ± 6 8 0.01 0.003

2. Cyflufenamid (F) 0.01 81 ± 9 20 0.01 0.003 117 ± 3 10 0.01 0.003

3. Amitraz (I) 0.01 41 ± 5 -35 0.01 0.003 41 ± 9 -26 0.01 0.003

4. Cyprodinil (F) 0.01 94 ± 9 23 0.009 0.003 86 ± 8 7 0.008 0.002

5. Mepanipirym (F) 0.01 85 ± 6 16 0.01 0.003 86 ± 6 7 0.01 0.003

6. Pyrimethanil (F) 0.01 85 ± 4 11 0.01 0.003 81 ± 6 4 0.008 0.002

7. Chlorantraniliprole1 (I) 0.01 86 ± 2 -56 0.01 0.003 64 ± 8 -15 0.01 0.003

8. Fenoxaprop-p-ethyl (H) 0.05 94 ± 9 6 0.03 0.009 72 ± 4 31 0.02 0.006

9. Fluazifop-p-butyl1 (H) 0.01 100 ± 8 51 0.03 0.009 124 ± 5 16 0.02 0.006

10. Propaquizafop (H) 0.05 107 ± 8 -26 0.03 0.009 87 ± 3 -11 0.03 0.009

11. Quizalofop-p-ethyl (H) 0.01 95 ± 4 7 0.01 0.003 93 ± 9 6 0.01 0.003

12. Fluopicolide (F) 0.01 85 ± 5 31 0.01 0.003 82 ± 2 8 0.01 0.003

13. Propyzamide (H) 0.01 93 ± 4 26 0.01 0.003 94 ± 5 11 0.01 0.003

14. Bromopropylate (A) 0.01 96 ± 5 121 0.01 0.003 120 ± 5 21 0.01 0.003

15. Fuberidazole (F) 0.01 n.d. 14 - - 43 ± 6 9 0.01 0.003

16. Thiabendazole (I) 0.01 n.d. 35 - - 43 ± 3 17 0.01 0.003

17. Dichlobenil (H) 0.01 86 ± 4 1 0.01 0.003 84 ± 5 1 0.01 0.003

18. Metrafenone (F) 0.01 107 ± 8 30 0.01 0.003 68 ± 2 4 0.009 0.003

19. Teflubenzuron (I) 0.05 109 ± 5 228 0.02 0.006 102 ± 6 49 0.02 0.006

20. Tetradifon (I) 0.01 91 ± 3 35 0.01 0.003 85 ± 5 10 0.01 0.003

21. Carbaryl1 (I) 0.01 88 ± 4 146 0.02 0.006 81 ± 5 169 0.01 0.003

22. Carbofuran1 (I) 0.01 85 ± 6 110 0.02 0.006 88 ± 2 215 0.01 0.003

23. Carbosulfan (I) 0.01 n.d. -40 - - 90 ± 5 -8 0.01 0.003

24. Chlorpropham (H) 0.05 94 ± 5 -112 0.01 0.003 120 ± 5 -17 0.01 0.003

25. Fenoxycarb (I) 0.01 98 ± 2 38 0.01 0.003 93 ± 5 95 0.01 0.003

26. Iprowalikarb (F) 0.05 82 ± 7 30 0.01 0.003 116 ± 5 25 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

MSPD QuEChERS

27. Isoprocarb (I) 0.01 97 ± 9 -77 0.01 0.003 92 ± 4 -30 0.01 0.003

28. Pirimicarb1.2 (I) 0.01 75 ± 8 -2 0.01 0.003 52 ± 7 -6 0.01 0.003

29. Pirimicarb desmethyl (I) 0.01 108 ± 18 10 0.01 0.003 79 ± 6 1 0.01 0.003

30. Propham (H) 0.05 77 ± 3 0.3 0.02 0.006 107 ± 6 1 0.01 0.003

31. Propoxur1 (I) 0.01 111 ± 1 -3 0.02 0.006 91 ± 4 -48 0.01 0.003

32. Boscalid (F) 0.01 86 ± 5 12 0.01 0.003 97 ± 3 2 0.008 0.002

33. Diflufenican (DFF) (H) 0.01 100 ± 9 166 0.01 0.003 120 ± 5 35 0.01 0.003

34. Hexythiazox (A) 0.05 69 ± 6 -50 0.04 0.012 93 ± 1 -19 0.04 0.012

35. Acetochlor (H) 0.01 83 ± 5 8 0.01 0.003 95 ± 4 8 0.01 0.003

36. Dimethenamid (H) 0.05 90 ± 6 66 0.02 0.006 71 ± 5 9 0.02 0.006

37. Metazachlor (H) 0.01 89 ± 3 26 0.01 0.003 84 ± 2 9 0.008 0.002

38. Metolachlor (H) 0.05 83 ± 15 2 0.02 0.006 109 ± 7 17 0.02 0.006

39. Propachlor (H) 0.05 80 ± 9 29 0.02 0.006 95 ± 5 17 0.02 0.006

40. Chlorothalonil1 (F) 0.01 92 ± 6 124 0.01 0.003 88 ± 4 23 0.01 0.003

41. Dicloran1 (F) 0.01 105 ± 3 -4 0.01 0.003 78 ± 3 -2 0.01 0.003

42. HCB (Hexachlorobenzene)1 (F)

0.01 81 ± 4 -45 0.005 0.001 84 ± 7 -11 0.005 0.001

43. Quintozene (PCNB) (F) 0.01 83 ± 6 3 0.01 0.003 84 ± 9 2 0.01 0.003

44. Tecnazene (TCNB) (F) 0.01 92 ± 9 7 0.009 0.003 105 ± 6 9 0.009 0.003

45. Tolclofos methyl (F) 0.01 75 ± 4 11 0.01 0.003 79 ± 5 10 0.01 0.003

46. Cymoxanil1 (F) 0.05 61 ± 3 30 0.04 0.012 72 ± 5 16 0.04 0.012

47. Iprodione1 (F) 0.05 101 ± 5 3161 0.02 0.006 112 ± 8 619 0.02 0.006

48. Procymidone (F) 0.01 106 ± 11 30 0.01 0.003 96 ± 16 9 0.01 0.003

49. Pendimethalin1 (H) 0.01 87 ± 8 15 0.01 0.003 92 ± 5 2 0.01 0.003

50. Trifluralin1 (H) 0.01 94 ± 1 7 0.01 0.003 98 ± 13 2 0.01 0.003

51. Nitrofen1 (H) 0.01 94 ± 3 -26 0.009 0.003 96 ± 4 -4 0.009 0.003

52. Oxyflurofen (H) 0.01 76 ± 7 14 0.009 0.003 101 ± 6 2 0.008 0.002

53. Fenhexamid (F) 0.05 97 ± 6 -44 0.02 0.006 76 ± 6 -91 0.02 0.006

54. Fenamidon (F) 0.01 102 ± 4 1 0.01 0.003 108 ± 7 18 0.01 0.003

55. Imazalil (F) 0.01 49 ± 5 5 0.02 0.006 44 ± 4 12 0.02 0.006

56. Prochloraz (F) 0.01 35 ± 3 -21 0.01 0.003 111 ± 8 -4 0.01 0.003

57. Triflumizole (F) 0.01 82 ± 6 35 0.02 0.006 74 ± 4 15 0.01 0.003

58. Isoxaflutole (H) 0.05 84 ± 5 30 0.02 0.006 95 ± 2 17 0.02 0.006

59. Clomazone1.2 (H) 0.01 73 ± 6 2 0.01 0.003 76 ± 5 2 0.01 0.003

60. Dimethomorph1 (F) 0.05 99 ± 3 -36 0.03 0.009 104 ± 1 -48 0.03 0.009

61. Fenpropimorph (F) 0.05 41 ± 9 3 0.02 0.006 92 ± 5 14 0.02 0.006

62. Acetamiprid1 (I) 0.01 41 ± 4 14 0.01 0.003 76 ± 5 14 0.01 0.003

63. Thiacloprid (I) 0.01 75 ± 3 15 0.01 0.003 71 ± 9 7 0.01 0.003

64. Thiametoxam1 (I) 0.01 62 ± 10 29 0.02 0.006 43 ± 2 3 0.01 0.003

65. Aldrine1 (I) 0.01 87 ± 7 -54 0.005 0.001 72 ± 8 -15 0.005 0.001

66. Alpha endosulfan1 (I) 0.01 89 ± 5 -7 0.008 0.002 87 ± 3 -18 0.007 0.002

ContinuedSupplementary Table 2: Validation parameters and matrix effect of MSPD and QuEChERS methods in tobacco studied by GC-µECD/NPD. Negative values of matrix effects mean suppression of the signal and positives values enhancement.

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

MSPD QuEChERS

67. Alpha HCH1 (I) 0.01 90 ± 6 -50 0.005 0.001 112 ± 9 -31 0.005 0.001

68. Beta endosulfan1 (I) 0.01 90 ± 8 -15 0.008 0.002 93 ± 3 -11 0.008 0.002

69. Beta HCH1 (I) 0.01 90 ± 6 -59 0.005 0.002 93 ± 5 -31 0.005 0.001

70. Dicofol (A) 0.01 82 ± 6 13 0.01 0.003 75 ± 6 2 0.009 0.003

71. Dieldrin1 (I) 0.01 95 ± 7 -56 0.005 0.001 84 ± 10 -18 0.005 0.001

72. Sulfate endosulfan1 (I) 0.01 96 ± 5 82 0.008 0.002 95 ± 4 10 0.008 0.002

73. Endrin1 (I) 0.01 110 ± 5 27 0.005 0.001 87 ± 13 28 0.005 0.001

74. Heptachlor1 (I) 0.01 92 ± 5 -27 0.005 0.001 76 ± 5 -3 0.005 0.001

75. Heptachlor epoxide1 (I) 0.01 95 ± 6 -55 0.005 0.001 81 ± 13 -20 0.005 0.001

76. Methoxychlor (DMDT)1 (I) 0.01 119 ± 6 1295 0.01 0.003 116 ± 3 14 0.01 0.003

77. o.p’-DDT1 (I) 0.01 120 ± 1 -79 0.005 0.001 115 ± 6 -22 0.005 0.001

78. p.p’-DDD1 (I) 0.01 104 ± 9 -76 0.005 0.001 102 ± 3 -20 0.005 0.001

79. p.p’-DDE1 (I) 0.01 91 ± 4 -56 0.005 0.001 83 ± 13 -21 0.005 0.001

80. p.p’-DDT1 (I) 0.01 125 ± 11 1148 0.005 0.001 115 ± 4 4 0.005 0.001

81. Azinphos ethyl1 (I) 0.01 87 ± 4 48 0.01 0.003 85 ± 3 30 0.01 0.003

82. Azinphos methyl1 (I) 0.01 84 ± 4 143 0.01 0.003 88 ± 9 47 0.01 0.003

83. Chlorfenvinphos1 (I) 0.01 82 ± 4 8 0.008 0.002 84 ± 4 7 0.008 0.002

84. Bromofos ethyl1 (I) 0.01 85 ± 3 10 0.009 0.003 78 ± 9 4 0.009 0.003

85. Bromofos methyl (I) 0.01 100 ± 6 9 0.009 0.003 86 ± 5 6 0.009 0.003

86. Cadusafos (I) 0.01 94 ± 9 20 0.008 0.002 104 ± 12 5 0.006 0.002

87. Chlorpyrifos1 (I) 0.01 90 ± 7 4 0.005 0.001 84 ± 4 1 0.005 0.001

88. Chlorpyrifos methyl1 (I) 0.01 88 ± 7 2 0.005 0.001 88 ± 8 5 0.005 0.001

89. Coumphos (I) 0.05 89 ± 5 52 0.03 0.009 80 ± 9 36 0.03 0.009

90. Diazinon1 (I) 0.01 81 ± 12 41 0.01 0.003 79 ± 6 5 0.01 0.003

91. Dichlorvos1 (I) 0.01 105 ± 14 90 0.01 0.003 95 ± 11 30 0.01 0.003

92. Dicrotophos (I) 0.01 61 ± 2 203 0.01 0.003 62 ± 9 42 0.01 0.003

93. Dimethoate1 (I) 0.01 104 ± 12 39 0.01 0.003 74 ± 2 25 0.01 0.003

94. EPN (I) 0.01 78 ± 10 23 0.008 0.002 85 ± 8 2 0.007 0.002

95. Ethion (I) 0.01 87 ± 6 27 0.008 0.002 92 ± 4 8 0.01 0.003

96. Ethoprophos1 (I) 0.01 112 ± 5 29 0.01 0.003 110 ± 6 9 0.01 0.003

97. Fenchlorfos1 (I) 0.01 76 ± 6 3 0.01 0.003 82 ± 7 5 0.01 0.003

98. Fenitrothion1 (I) 0.01 91 ± 9 12 0.01 0.003 85 ± 9 2 0.009 0.003

99. Fention1 (I) 0.01 74 ± 5 25 0.01 0.003 80 ± 4 5 0.01 0.003

100. Formothion1 (I) 0.01 104 ± 4 9 0.01 0.003 109 ± 5 2 0.01 0.003

101. Fostiazate (I) 0.01 97 ± 2 142 0.01 0.003 82 ± 3 41 0.008 0.002

102. Heptenophos (I) 0.01 78 ± 2 57 0.01 0.003 79 ± 6 13 0.01 0.003

103. Isocarbophos (A) 0.01 90 ± 3 83 0.01 0.003 93 ± 10 69 0.01 0.003

104. Isofenphos (I) 0.01 91 ± 4 55 0.01 0.003 84 ± 8 11 0.01 0.003

105. Isofenfos methyl (I) 0.01 88 ± 16 41 0.01 0.003 78 ± 8 7 0.01 0.003

106. Malaoxon (I) 0.01 99 ± 4 44 0.01 0.003 71 ± 7 20 0.01 0.003

107. Malathion1 (I) 0.01 90 ± 13 80 0.01 0.003 93 ± 6 22 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

MSPD QuEChERS

108. Mecarbam (I) 0.01 89 ± 3 -1 0.01 0.003 80 ± 2 7 0.01 0.003

109. Methacrifos (F) 0.01 84 ± 3 30 0.01 0.003 88 ± 8 4 0.01 0.003

110. Methidathion1 (I) 0.01 76 ± 4 21 0.01 0.003 72 ± 1 9 0.01 0.003

111. Mevinphos (I) 0.01 92 ± 6 37 0.01 0.003 81 ± 14 14 0.01 0.003

112. Paraoxon ethyl (I) 0.01 83 ± 6 -14 0.01 0.003 79 ± 7 -12 0.009 0.003

113. Paraoxon methyl (I) 0.01 83 ± 13 78 0.01 0.003 78 ± 9 61 0.009 0.003

114. Parathion ethyl1 (I) 0.01 86 ± 5 7 0.01 0.003 80 ± 8 3 0.009 0.003

115. Parathion methyl1 (I) 0.01 81 ± 4 9 0.01 0.003 81 ± 9 7 0.009 0.003

116. Phentoate (I) 0.01 81 ± 6 61 0.01 0.003 79 ± 7 1 0.01 0.003

117. Phorate1 (I) 0.01 86 ± 5 50 0.01 0.003 116 ± 5 29 0.01 0.003

118. Phosalone1 (I) 0.01 97 ± 15 25 0.01 0.003 85 ± 11 3 0.01 0.003

119. Phosmet (I) 0.01 93 ± 13 102 0.01 0.003 111 ± 3 30 0.01 0.003

120. Pirimiphos ethyl (I) 0.01 74 ± 6 49 0.009 0.003 79 ± 4 5 0.009 0.003

121. Pirimiphos methyl1 (I) 0.01 75 ± 5 35 0.009 0.003 87 ± 8 4 0.009 0.003

122. Profenofos1 (I) 0.01 81 ± 6 42 0.01 0.003 81 ± 4 25 0.01 0.003

123. Quinalphos (I) 0.01 83 ± 3 31 0.008 0.002 79 ± 7 4 0.007 0.002

124. Tetrachlorwinfos1 (I) 0.01 86 ± 15 157 0.01 0.003 90 ± 11 45 0.008 0.002

125. Triazophos (I) 0.01 77 ± 9 62 0.01 0.003 92 ± 8 23 0.01 0.003

126. Indoxacarb1 (I) 0.01 86 ± 6 -22 0.01 0.003 112 ± 6 -26 0.01 0.003

127. Flutolanil (F) 0.05 70 ± 3 258 0.03 0.009 97 ± 6 1 0.02 0.006

128. Famoksadone1 (F) 0.05 82 ± 6 30 0.01 0.003 78 ± 5 25 0.01 0.003

129. Vinclozolin (F) 0.01 93 ± 14 4 0.01 0.003 82 ± 4 1 0.01 0.003

130. Chlozolinate (F) 0.01 92 ± 3 -8 0.01 0.003 75 ± 5 -6 0.01 0.003

131. Flufenacet (H) 0.01 91 ± 15 19 0.01 0.003 95 ± 12 2 0.01 0.003

132. Benalaxyl1 (F) 0.01 90 ± 6 13 0.01 0.003 117 ± 4 50 0.01 0.003

133. Metalaxyl1.2 (F) 0.01 61 ± 4 123 0.01 0.003 90 ± 10 0.4 0.01 0.003

134. Oksadixyl1 (F) 0.01 96 ± 5 8 0.01 0.003 90 ± 7 24 0.01 0.003

135. Fipronil (I) 0.01 76 ± 16 364 0.009 0.003 80 ± 7 57 0.009 0.003

136. Fluazinam (F) 0.01 101 ± 2 -22 0.01 0.003 82 ± 4 -28 0.01 0.003

137. Fludioxonil (F) 0.01 91 ± 4 -18 0.01 0.003 98 ± 5 -2 0.01 0.003

138. Pencycuron (F) 0.05 85 ± 4 -71 0.02 0.006 85 ± 8 -9 0.01 0.003

139. Isoprothiolane (F) 0.01 87 ± 5 12 0.01 0.003 102 ± 4 15 0.01 0.003

140. Pyrazofos (I) 0.01 103 ± 8 44 0.01 0.003 76 ± 7 13 0.01 0.003

141. Captafol (F) 0.01 79 ± 11 965 0.01 0.003 71 ± 8 765 0.01 0.003

142. Captan1 (F) 0.01 89 ± 13 1874 0.01 0.003 96 ± 3 1101 0.01 0.003

143. Folpet1 (F) 0.01 87 ± 2 85 0.01 0.003 85 ± 5 25 0.01 0.003

144. Tebufenpyrad (A) 0.01 79 ± 4 -7 0.01 0.003 80 ± 5 -3 0.01 0.003

145. Acrinathrin (I) 0.01 62 ± 4 716 0.01 0.003 86 ± 8 66 0.01 0.003

146. Bifenthrin1 (I) 0.01 67 ± 6 74 0.01 0.003 75 ± 5 5 0.01 0.003

147. Cyfluthrin1 (I) 0.05 95 ± 8 161 0.02 0.006 85 ± 4 33 0.02 0.006

148. Cypermethrin1.2 (I) 0.05 109 ± 13 -113 0.01 0.003 97 ± 12 -30 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

MSPD QuEChERS

149. Deltamethrin1 (I) 0.05 110 ± 10 39 0.01 0.003 90 ± 14 11 0.01 0.003

150. Esfenvalerate1 (I) 0.01 90 ± 5 80 0.01 0.003 100 ± 5 14 0.01 0.003

151. Fenpropathrin (I) 0.01 100 ± 1 4 0.01 0.003 105 ± 5 1 0.01 0.003

152. Fenvalerate1 (I) 0.01 92 ± 5 -21 0.01 0.003 86 ± 11 -20 0.01 0.003

153. Gamma HCH (Lindane)1 (I) 0.01 96 ± 11 -50 0.005 0.001 88 ± 3 -17 0.005 0.001

154. Lambda cyhalothrin1 (I) 0.01 82 ± 5 99 0.01 0.003 81 ± 7 8 0.01 0.003

155. Permethrin1 (I) 0.05 96 ± 5 225 0.04 0.012 114 ± 54 21 0.03 0.009

156. Pyrethrin1 (I) 0.05 90 ± 6 25 0.04 0.012 64 ± 8 16 0.03 0.009

157. Tau-Fluvalinate (I) 0.01 92 ± 13 379 0.01 0.003 83 ± 11 284 0.009 0.003

158. Tefluthrin1 (I) 0.01 84 ± 8 9 0.009 0.003 89 ± 1 6 0.007 0.002

159. Tetramethrin (I) 0.05 91 ± 3 657 0.03 0.009 86 ± 2 137 0.02 0.006

160. Zoxamide (F) 0.01 113 ± 5 -48 0.009 0.003 73 ± 5 -76 0.007 0.002

161. Chloridazon (H) 0.01 87 ± 3 -1 0.009 0.003 44 ± 4 -15 0.007 0.002

162. Flurtamone (H) 0.01 89 ± 9 -10 0.01 0.003 88 ± 6 -5 0.009 0.003

163. Pyridaben (A) 0.05 90 ± 4 375 0.02 0.006 82 ± 7 3 0.01 0.003

164. Flonicamid (I) 0.01 42 ± 5 -1 0.01 0.003 46 ± 4 -1 0.01 0.003

165. Fenarimol (F) 0.01 97 ± 3 23 0.01 0.003 81 ± 14 6 0.009 0.003

166. Bupirimate (F) 0.01 103 ± 6 10 0.01 0.003 61 ± 6 5 0.007 0.002

167. Quinoxyfen (F) 0.01 98 ± 6 12 0.009 0.003 111 ± 5 16 0.008 0.002

168. Azoxystrobin (F) 0.01 83 ± 5 -19 0.01 0.003 73 ± 1 -3 0.01 0.003

169. Dimoksystrobina (F) 0.01 86 ± 12 123 0.01 0.003 78 ± 6 20 0.01 0.003

170. Fluoxastrobin (F) 0.01 105 ± 19 1025 0.01 0.003 100 ± 13 57 0.01 0.003

171. Kresoxim methyl (F) 0.01 99 ± 7 31 0.01 0.003 87 ± 7 4 0.008 0.002

172. Picoxystrobin (F) 0.05 104 ± 6 -4 0.03 0.009 90 ± 3 -3 0.01 0.003

173. Pyraklostrobina (F) 0.05 91 ± 4 32 0.05 0.015 91 ± 3 29 0.05 0.015

174. Trifloxystrobin (F) 0.01 104 ± 2 18 0.01 0.003 101 ± 10 13 0.007 0.002

175. Propargite (A) 0.05 59 ± 6 363 0.05 0.015 128 ± 14 252 0.05 0.015

176. Tritosulfuron (H) 0.01 86 ± 5 78 0.01 0.003 90 ± 3 56 0.009 0.003

177. Dichlofluanid (F) 0.01 91 ± 8 20 0.01 0.003 86 ± 12 0.4 0.01 0.003

178. Tolylfluanid (F) 0.01 94 ± 7 31 0.01 0.003 84 ± 5 8 0.01 0.003

179. Spirodiclofen (A) 0.01 90 ± 9 -7 0.01 0.003 92 ± 5 -11 0.008 0.002

180. Atrazine (H) 0.01 81 ± 5 13 0.01 0.003 82 ± 3 13 0.009 0.003

181. Cyanazine (H) 0.01 80 ± 5 3 0.01 0.003 77 ± 3 10 0.009 0.003

182. Cyprazine (H) 0.01 78 ± 3 9 0.01 0.003 104 ± 4 9 0.009 0.003

183. Procyazine (H) 0.01 124 ± 12 -4 0.01 0.003 110 ± 6 -30 0.009 0.003

184. Prometrine (H) 0.01 73 ± 10 10 0.01 0.003 82 ± 5 16 0.009 0.003

185. Propazine (H) 0.01 85 ± 10 5 0.01 0.003 92 ± 13 5 0.009 0.003

186. Simazine (H) 0.01 72 ± 6 2 0.01 0.003 78 ± 2 2 0.008 0.002

187. Terbuthylazine (H) 0.01 118 ± 17 5 0.009 0.003 87 ± 9 3 0.009 0.003

188. Terbutryn (H) 0.01 67 ± 8 0.4 0.009 0.003 77 ± 4 1 0.009 0.003

189. Metamitron (H) 0.01 60 ± 9 128 0.01 0.003 108 ± 6 10 0.01 0.003

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

Matrix effect (%)

LOQ(mg/kg)

LOD (mg/kg)

MSPD QuEChERS

190. Metribuzin (H) 0.01 85 ± 6 5 0.009 0.003 77 ± 7 5 0.009 0.003

191. Azaconazole (F) 0.01 120 ± 5 -4 0.01 0.003 102 ± 11 12 0.008 0.002

192. Bitertanol (F) 0.05 57 ± 2 23 0.02 0.006 89 ± 15 24 0.01 0.003

193. Bromuconazole (F) 0.01 108 ± 1 213 0.01 0.003 91 ± 6 8 0.01 0.003

194. Cyproconazole (F) 0.01 82 ± 7 -28 0.01 0.003 74 ± 4 -6 0.01 0.003

195. Difenoconazole (F) 0.05 55 ± 2 -17 0.01 0.003 76 ± 9 -23 0.01 0.003

196. Dinikonazol (F) 0.01 96 ± 7 6 0.009 0.003 85 ± 11 20 0.008 0.002

197. Epoxiconazole (F) 0.01 92 ± 7 102 0.009 0.003 110 ± 6 16 0.009 0.003

198. Etaconazole (F) 0.01 69 ± 14 -10 0.01 0.003 89 ± 14 -1 0.009 0.003

199. Fenbuconazole (F) 0.01 49 ± 6 -12 0.01 0.003 77 ± 2 -8 0.01 0.003

200. Fluquinconazole (F) 0.01 80 ± 6 3 0.01 0.003 74 ± 2 2 0.008 0.002

201. Flusilazole (F) 0.01 60 ± 6 18 0.009 0.003 91 ± 14 14 0.008 0.002

202. Flutriafol (F) 0.05 43 ± 5 -23 0.02 0.006 57 ± 6 18 0.01 0.003

203. Hexaconazole (F) 0.01 102 ± 8 17 0.009 0.003 82 ± 12 5 0.009 0.003

204. Imibenkonazol (F) 0.01 60 ± 13 -36 0.01 0.003 71 ± 5 -41 0.008 0.002

205. Metkonazol (F) 0.05 63 ± 8 38 0.02 0.006 87 ± 7 31 0.01 0.003

206. Myclobutanyl (F) 0.01 103 ± 5 18 0.01 0.003 90 ± 11 13 0.009 0.003

207. Paclobutrazol (F) 0.01 74 ± 5 -14 0.01 0.003 70 ± 5 -2 0.01 0.003

208. Penconazole1 (F) 0.01 62 ± 7 18 0.009 0.003 80 ± 17 7 0.008 0.002

209. Propiconazole (F) 0.01 76 ± 9 8 0.01 0.003 86 ± 4 13 0.01 0.003

210. Prothioconazole (F) 0.01 45 ± 15 16 0.01 0.003 86 ± 3 8 0.01 0.003

211. Tebuconazole (F) 0.01 50 ± 9 12 0.01 0.003 124 ± 4 30 0.009 0.003

212. Tetraconazole (F) 0.01 60 ± 5 18 0.01 0.003 75 ± 18 1 0.009 0.003

213. Triadimefon (F) 0.01 0.008 6 0.01 0.003 0.008 4 0.01 0.003

214. Triadimenol (F) 0.05 74 ± 7 22 0.03 0.009 83 ± 9 5 0.01 0.003

215. Triticonazole (F) 0.01 87 ± 6 -7 0.01 0.003 115 ± 5 -2 0.01 0.003

216. Buprofezin (I) 0.01 83 ± 8 77 0.01 0.003 88 ± 3 11 0.01 0.003

217. DEET N.N-dietylo-m-toluamid (I)

0.05 84 ± 7 197 0.03 0.009 95 ± 4 30 0.01 0.003

218. Difenyloamina (F) 0.01 82 ± 8 -6 0.01 0.003 96 ± 6 -1 0.01 0.003

219. Fenazaquin (I) 0.01 95 ± 4 13 0.01 0.003 111 ± 5 69 0.01 0.003

220. Flurochloridone (H) 0.01 76 ± 5 15 0.009 0.003 112 ± 10 3 0.006 0.002

221. Pyriproxyfen (I) 0.05 88 ± 3 35 0.02 0.006 85 ± 5 23 0.01 0.003

222. Quinoclamine (H) 0.01 90 ± 5 81 0.01 0.003 84 ± 12 11 0.009 0.003

223. Lenacil (H) 0.05 90 ± 3 342 0.02 0.006 95 ± 11 329 0.01 0.003

*LOQ - Limit of quantification**LOD - Limit of detection1 List of the pesticides employed for tobacco (CORESTA)2 Pesticides recommended for tobacco cultivationn.d. not detected

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