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Chromatographic integration Mandatory ‣ Chromatograms must be visually inspected ‣ Consistent approach must be adopted ( Capability of instrument) ‣ Chromatographic integration and baseline adjustment Characterization ‣ Characteristic ion chromatograms ‣ Selectivity ‣ Compromise to integrate in one step ‣ List of Residue amenable one by one 16 Guy Jamet – STRBG
Performance-criteria qualitative screening method validation Mandatory Characterization ‣ Low probability of presence ‣ Confidence established at a certain concentration level ‣ Representative of for the matrix scope ‣ No regard of linearity and recovery ‣ False positive excluded with blank samples ‣ Repeatability of presence ‣ Depending if method is conducted in solvent or matrix ‣ All residues ‣ Confidence by repeatability of quantification when MS spectra is amenable ‣ False positive from past injection must be avoided 17 Guy Jamet – STRBG
Page 1 and 2: Guy JAMET PhD SCL: Service Commun d
Page 3 and 4: Organisation of plant protection
Page 5 and 6: The controls ‣ Official labs depe
Page 7 and 8: Requirements of labs dealing with P
Page 9 and 10: Sanco mandatory and possible applic
Page 11 and 12: Standards Mandatory Characterizatio
Page 13 and 14: Sequences Mandatory ‣ Length of t
Page 15: Matrix effect Mandatory ‣ Differe
Page 19 and 20: Acceptability of analytical perform
Page 21 and 22: Confirmation results Mandatory ‣
Page 23 and 24: Reporting results Mandatory Charact
Page 25 and 26: Statistical tools 25 Guy Jamet - ST
Page 27 and 28: 27 Guy Jamet - STRBG NF V03-110 as
Page 29 and 30: Homogeneity, stability Real sample
Page 31 and 32: Variability Precision and accuracy
Page 33 and 34: 33 Guy Jamet - STRBG NF V03-110 as
Page 35 and 36: 35 Guy Jamet - STRBG Historical kno
Page 37 and 38: 37 Guy Jamet - STRBG The different
Page 39 and 40: Avoiding contamination ‣ Premises
Page 41 and 42: Control at reception ‣ Mandatory
Page 43 and 44: 43 Guy Jamet - STRBG Amenable Essay
Page 45 and 46: Carry out of the GC/MS extract ‣
Page 47 and 48: Interpretation of the data ‣ Qual
Page 49 and 50: Capability of acting people ‣Samp
Page 51 and 52: Characterization of the MS ‣ MS p
Page 53 and 54: Characterization of standards ‣ I
Page 55 and 56: Explanation of a spectra O O N Cl N
Page 57 and 58: 57 Guy Jamet - STRBG 1 st step of t
Page 59 and 60: 59 Guy Jamet - STRBG Working plan
Page 61 and 62: 61 Guy Jamet - STRBG 2 nd Proposal
Page 63 and 64: 63 Guy Jamet - STRBG Instrument res
Page 65 and 66: 65 Guy Jamet - STRBG CYPRODINIL (LC
Page 67 and 68:
67 Guy Jamet - STRBG λ CYHALOTHRIN
Page 69 and 70:
69 Guy Jamet - STRBG IPRODIONE (LCL
Page 71 and 72:
71 Guy Jamet - STRBG PYRIMETHANIL (
Page 73 and 74:
73 Guy Jamet - STRBG Conclusion on
Page 75 and 76:
75 Guy Jamet - STRBG Instrument dev
Page 77 and 78:
Response CHLORFENVINPHOS (Cal) Chlo
Page 79 and 80:
CYPRODINIL (Cal) Cyprodinil ppb Min
Page 81 and 82:
Response 81 Guy Jamet - STRBG CYPRO
Page 83 and 84:
Response ETHION (Cal) Ethion 600000
Page 85 and 86:
OXADIXYL (Cal) Oxadixyl ppb Min Mea
Page 87 and 88:
Response OXADIXYL (Cal) Oxadixyl (I
Page 89 and 90:
Response 89 Guy Jamet - STRBG IPROD
Page 91 and 92:
PROCYMIDONE (Cal) Procymidone ppb M
Page 93 and 94:
Response 93 Guy Jamet - STRBG PROCY
Page 95 and 96:
Response 95 Guy Jamet - STRBG PYRIM
Page 97 and 98:
λ CYHALOTHRIN (Cal) λ Cyhalothrin
Page 99 and 100:
Response λ CYHALOTHRIN (Cal) λ Cy
Page 101 and 102:
Response 101 Guy Jamet - STRBG TOLC
Page 103 and 104:
VINCLOZOLINE (Cal) Vinclozoline ppb
Page 105 and 106:
Response VINCLOZOLINE (Cal) Vincloz
Page 107 and 108:
107 Guy Jamet - STRBG Calibration i
Page 109 and 110:
109 Guy Jamet - STRBG CYPRODINIL (L
Page 111 and 112:
111 Guy Jamet - STRBG λ CYHALOTHRI
Page 113 and 114:
113 Guy Jamet - STRBG PYRIMETHANIL
Page 115 and 116:
115 Guy Jamet - STRBG TOLCLOPHOS ME
Page 117 and 118:
117 Guy Jamet - STRBG CHLORFENVINPH
Page 119 and 120:
119 Guy Jamet - STRBG IPRODIONE (AC
Page 121 and 122:
121 Guy Jamet - STRBG PROCYMIDONE (
Page 123 and 124:
123 Guy Jamet - STRBG TOLCLOPHOS ME
Page 125 and 126:
125 Guy Jamet - STRBG VINCLOZOLINE
Page 127 and 128:
127 Guy Jamet - STRBG 3 rd proposal
Page 129 and 130:
129 Guy Jamet - STRBG IPRODIONE (hi
Page 131 and 132:
131 Guy Jamet - STRBG PYRIMETHANIL
Page 133 and 134:
133 Guy Jamet - STRBG Extension to
Page 135 and 136:
Mean, bias, RSD_r, RSD_FI (3) Resid
Page 137 and 138:
Mean, bias, RSD_r, RSD_FI (5) Resid
Page 139 and 140:
LOQ, LOD, LMR (1) C_100 C_200 C_500
Page 141 and 142:
Capability of determination (2) Res
Page 143 and 144:
143 Guy Jamet - STRBG 13 analytes w
Page 145 and 146:
145 Guy Jamet - STRBG 20 analytes w
Page 147 and 148:
147 Guy Jamet - STRBG SUMMARY ‣ 6
Page 149 and 150:
149 Guy Jamet - STRBG CHLORPYRIPHOS
Page 151 and 152:
151 Guy Jamet - STRBG Residues not
Page 153 and 154:
Residues amenable for every matrice
Page 155 and 156:
Prediction of the proficiency testi
Page 157 and 158:
Z-score EUPT 157 Guy Jamet - STRBG
Page 159 and 160:
Z-score EUPT by analytes and differ
Page 161 and 162:
4,4' DDE 1963 0,164 0,187 Azinphos
Page 163 and 164:
Decision of the scope ‣ Sequence
Page 165 and 166:
Variability OPP Dip Chl Dim Pro Pyr
Page 167 and 168:
Variability Imazalil Fludixonyl End
Page 169 and 170:
169 Guy Jamet - STRBG Deviation Pyr
Page 171 and 172:
Response 171 Guy Jamet - STRBG Prof
Page 173 and 174:
Response 173 Guy Jamet - STRBG Prof
Page 175 and 176:
175 Guy Jamet - STRBG Repeatability
Page 177 and 178:
177 Guy Jamet - STRBG On going cont
Page 179 and 180:
On going control Sequence : 11/03/0
Page 181 and 182:
181 Guy Jamet - STRBG 2 nd step of
Page 183 and 184:
183 Guy Jamet - STRBG Low and excee
Page 185 and 186:
Unexplainable recoveries on apples
Page 187 and 188:
187 Guy Jamet - STRBG Recoveries on
Page 189 and 190:
189 Guy Jamet - STRBG Recoveries on
Page 191 and 192:
Dossier of validation for GC-MS 191
Page 193 and 194:
193 Guy Jamet - STRBG Validation fo
Page 195 and 196:
Working plan for the determination
Page 197 and 198:
Response (area) 197 Guy Jamet - STR
Page 199 and 200:
Predicted concentrations 199 Guy Ja
Page 201 and 202:
201 Guy Jamet - STRBG CARBENDAZIME
Page 203 and 204:
203 Guy Jamet - STRBG Fitting and r
Page 205 and 206:
205 Guy Jamet - STRBG Layout of Rep
Page 207 and 208:
207 Guy Jamet - STRBG Results of Re
Page 209 and 210:
Dossier of validation for LC-MS/MS
Page 211:
211 Guy Jamet - STRBG Thank you for
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