Peer validation of Trifloxystrobin Impurity CGA 344605
"Explore the peer validation process for the relevant impurity CGA 344605 in trifloxystrobin formulations. Learn about the method, participants, and details of CGA 344605 determination. Detailed information on trifloxystrobin and its relevant impurity presented. Discover the outline and method parameters for accurate analysis. Peer validation conducted by key industry players for quality assurance. Visit for comprehensive insights on trifloxystrobin validation in June 2021."
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Trifloxystrobin Rel. Impurity CGA 344605 Peer Validation /////////// June 2021, CIPAC Friedhelm Schulz Bayer AG Research & Development, Crop Science
Background and Objective Background Peer validation for the relevant impurity CGA 344605 of the active substance trifloxystrobin in formulaitons was performed Objective Presentation of the outcome of the peer validation of Method CIPAC/5289/m, suitable for the determination of CGA 344605 in trifloxystrobin TC and trifloxystrobin EC, SC and WG formulations 2 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Participants BASF Bayer FFM Bayer Monheim Syngenta Currenta 3 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
TRIFLOXYSTROBIN ISO common name: trifloxistrobin Chemical name: methyl (E)-methoxyimino-{(E)- -[1-( , , -trifluoro-m- tolyl)ethylideneaminooxy]-o-tolyl}acetate (ISO) CAS-No.: 141517-21-7 CH3 Structure: O H3 N C F O O F CH3 N F O Empirical formula: Molecular mass: Relevante impurity: C20H19F3N2O4 408.37 g/mol CGA 344605, maximal accepted limit (MAL): 0.4% in TC 4 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
TRIFLOXYSTROBIN, relevant impurity CGA 344605 ISO common name: CGA 344605 Chemical name: methyl (E)-(2-chloromethylphenyl)-methoxy-imino-acetate CAS-No.: 189813-45-4 Structure: Empirical formula: Molecular mass: C11H12Cl1N1O3 241.68 g/mol 5 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Outline of the Method and Samples The content of CGA 344605 (% w/w) is determined by reversed phase high performance liquid chromatography using UV detection and external standard calibration. Samples: trifloxystrobin TC trifloxystrobin WG 50 (500 g/kg) fluoxastrobin + prothioconazole + trifloxystrobin EC 300 (75+150+75 g/L ) trifloxystrobin SC 500 (500 g/L ) 6 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Outline of the Method Method Parameters: Column: Ascentis Express C18 18; 2.7 m, 100 x 4.6 mm 35 C Column temperature: Time [min] water + 0.1 phosphoric acid [%v/v] 54 40 05 05 54 54 ACN + 0.1 phosphoric acid [%v/v] 46 60 95 95 46 46 Flow rate [mL/min] Eluent & rinsing gradiend 1.8 1.8 1.8 1.8 1.8 1.8 0.0 6.0 6.2 8.0 8.2 13 Injection volume: Retention time: Detector: 5 L approx. 1.7 min DAD, 210 nm 7 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Spectra Reference Item UV-Spectra 8 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Typical Chromatograms Analytical standard CGA 344605 (nominal 0.2 mg/50 mL - acetonitrile) 9 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Typical Chromatograms Analytical standard CGA 344605 (nominal 0.2 mg/50 mL acetonitrile/water) 10 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Typical Chromatograms Tryfloxystrobin TC/EC/WG/SC spiked with CGA 344605 SC 500 TC EC 300 WG 500 11 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical evaluation Statistical evaluation was performed based on the data of 5 participants. The investigared items are: Specificity and Interferences Linearity Precision Accuracy (Level I & Level II) LOQ 12 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical evaluation Identity: The UV spectra of standard and spiked sample solutions were measured under the operating conditions of the method. Specificity:Interferences at the retention time of the analyte in the technical material and in the formulations were checked by comparing the chromatograms of the reference standard CGA 344605 and the test solutions of technical material, formulations and blank formulations. The specificity of the analytical method for CGA 344605 is assessed sufficient as no significant interfering compounds were detected in the chromatograms at the retention time of the analyte. 13 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical evaluation Linearity, developing lab in acetonitrile/water in acetonitrile Number of values Regression equation n = 8 y = a + b x Number of values Regression equation n = 8 y = a + b x (1st order) (1st order) y = -0.000678 + 3.105749 x = 0.99995 y = 0.000502 + 3.070411 x = 0.99996 Correlation coefficient Correlation coefficient 14 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical evaluation Linearity (in acetonitrile), developing lab 1-4 Lab 1 Lab 2 Correlation coefficient = 0.99998 Correlation coefficient = 0.99998 Lab 4 Lab 3 Correlation coefficient = 0.99997 Correlation coefficient = 0.99982 15 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical evaluation Linearity (in acetonitrile/water), developing lab 1-4 Lab 2Lab 2 Lab 1 Lab 2 Correlation coefficient = 0.99997 Correlation coefficient = 0.99991 Lab 4 Lab 3 Correlation coefficient = 0.99999 Correlation coefficient = 0.99992 16 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary - Repeatability Triflosxystrobin TC (spiked with CGA 344605) CGA 344605 [mg/50 mL] Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 0.1107 0.1093 0.1020 0.1102 Weighing no. 1 0.1026 0.1085 0.1087 0.1019 0.1098 Weighing no. 2 0.1031 0.1010 0.1097 0.1021 0.1101 Weighing no. 3 0.1026 0.1104 0.1081 0.1022 0.1101 Weighing no. 4 0.1026 0.1078 0.1090 0.1027 0.1104 Weighing no. 5 0.1040 0.1131 0.1089 0.1021 0.1104 Weighing no. 6 0.1031 0.110 0.109 0.103 0.102 0.110 Mean value [mg/50 mL] 0.220 0.218 0.206 0.204 0.220 Mean value [% w/w] 0.00186 0.000543 0.000548 0.00028 0.000225 SD 1.69 0.50 0.54 0.27 0.20 RSD [%] 3.37 3.37 3.40 3.40 3.37 Horwitz-Value RSD (r)max 0.50 0.15 0.16 0.08 0.06 Horrat value Hr no no yes* no no Outliers *Not taken into account all values were calculated 17 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary - Repeatability Triflosxystrobin TC SC 500 (500 g/L) (spiked with CGA 344605) CGA 344605 [mg/50 mL] Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 0.1060 0.1062 0.1003 0.0995 0.1068 Weighing no. 1 0.1071 0.1066 0.0996 0.0996 0.1070 Weighing no. 2 0.1053 0.106 0.0981 0.0993 0.1076 Weighing no. 3 0.1044 0.1065 0.1029 0.0994 0.1069 Weighing no. 4 0.1055 0.1059 0.0995 0.0995 0.1073 Weighing no. 5 0.1054 0.1059 0.0989 0.0994 0.1055 Weighing no. 6 0.106 0.106 0.0999 0.0995 0.107 Mean value [mg/50 mL] 0.0918 0.0918 0.0869 0.0865 0.0929 Mean value [% w/w] 0.000906 0.000306 0.00165 0.000105 0.000723 SD 0.86 0.29 1.65 0.11 0.68 RSD [%] 3.84 3.84 3.87 3.87 3.83 Horwitz-Value RSD (r)max 0.22 0.08 0.43 0.03 0.18 Horrat value Hr no no no no no Outliers 18 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary - Repeatability fluoxastrobin+prothioconazole+triflosxystrobin EC 300 (75+150+75 g/L) (spiked with CGA 344605) CGA 344605 [mg/50 mL] Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 0.1124 0.1004 0.0934 0.0932 0.1098 Weighing no. 1 0.1001 0.1018 0.0908 0.0934 0.1027 Weighing no. 2 0.1036 0.0991 0.0903 0.0941 0.1034 Weighing no. 3 0.1025 0.0999 0.0908 0.0936 0.1026 Weighing no. 4 0.1026 0.1043 0.0932 0.0936 0.1029 Weighing no. 5 0.1034 0.0984 0.0907 0.0935 0.1026 Weighing no. 6 0.102 0.101 0.0915 0.0936 0.103 Mean value [mg/50 mL] 0.0133 0.0131 0.0119 0.0122 0.0134 Mean value [% w/w] 0.00137 0.00213 0.00138 0.000301 0.000336 SD 1.34 2.12 1.51 0.32 0.33 RSD [%] 5.13 5.15 5.22 5.21 5.13 Horwitz-Value RSD (r)max 0.26 0.41 0.29 0.06 0.06 Horrat value Hr Yes* no no no Yes* Outliers *outlier taken into account, the values were disregarded CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations 19
Statistical Summary - Repeatability Triflosxystrobin WG 50 (500 g/kg) (spiked with CGA 344605) CGA 344605 [mg/50 mL] Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 0.1115 0.1077 0.1040 0.1031 0.1105 Weighing no. 1 0.1095 0.1059 0.1039 0.1033 0.1111 Weighing no. 2 0.1099 0.1057 0.1036 0.1034 0.1102 Weighing no. 3 0.1096 0.1049 0.1022 0.1037 0.1112 Weighing no. 4 0.1095 0.1051 0.1022 0.1053 0.1090 Weighing no. 5 0.1088 0.1041 0.1020 0.1040 0.1107 Weighing no. 6 0.110 0.106 0.103 0.104 0.110 Mean value [mg/50 mL] 0.110 0.106 0.103 0.104 0.110 Mean value [% w/w] 0.000919 0.00122 0.000943 0.0008 0.000802 SD 0.84 1.16 0.92 0.77 0.73 RSD [%] 3.74 3.76 3.77 3.77 3.73 Horwitz-Value RSD (r)max 0.22 0.31 0.24 0.20 0.20 Horrat value Hr no no no no no Outliers 20 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary Recovery Level I + II Triflosxystrobin TC CGA 344605 Recovery [%] Recovery Level I - LOQ Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Mean value 100.4 104.8 96.6 98.9 99.5 1.55 1.31 1.52 0.71 0.72 SD 1.54 0.96 1.57 0.72 0.73 RSD [%] no no Yes* no Yes* Outliers CGA 344605 Recovery [%] Recovery Level II - MAL Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Mean value 101.4 103.3 100.6 100.9 100.4 0.58 0.23 0.37 0.15 0.09 SD 0.57 0.23 0.36 0.15 0.09 RSD [%] no no no no no Outliers *Not taken into account all values were calculated 21 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary Recovery Level I + II Triflosxystrobin SC 500 (500 g/L) CGA 344605 Recovery Level I - LOQ Recovery [%] Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Mean value 100.7 98.2 94.2 100.3 97.8 2.33 0.894 0.659 0.764 2.80 SD 2.31 0.91 0.70 0.76 2.86 RSD [%] no no no no yes* Outliers CGA 344605 Recovery [%] Recovery Level II - MAL Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 99.2 Mean value 100.4 99.6 98.6 97.4 0.14 0.60 0.47 0.09 0.54 SD 0.14 0.60 0.48 0.09 0.55 RSD [%] no no no no yes* Outliers *Not taken into account all values were calculated 22 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary Recovery Level I + II fluoxastrobin+prothioconazole+triflosxystrobin EC 300 (75+150+75 g/L) *Not taken into account all values were calculated CGA 344605 Recovery [%] Recovery Level I - LOQ Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Mean value 97.5 108.9 85.7 93.4 95.4 2.28 3.66 1.45 0.45 2.64 SD 2.34 3.58 1.70 0.48 2.77 RSD [%] yes* no no no no Outliers *outlier taken into account, the values were disregarded CGA 344605 Recovery [%] Recovery Level II - MAL Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Weighing no. 6 100.0 100.7 97.76 97.32 96.91 99.4 101.1 98.3 97.3 96.7 Mean value 0.66 0.31 0.62 0.14 0.53 SD 0.67 0.31 0.63 0.14 0.54 RSD [%] no no yes** no yes** Outliers **Not taken into account all values were calculated 23 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical Summary Recovery Level I + II Triflosxystrobin WG 50 (500 g/kg) CGA 344605 Recovery Level I - LOQ Recovery [%] Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Mean value 100.3 77.9 94.7 97.9 111.1 3.81 4.56 1.08 4.06 3.87 SD 3.66 5.85 1.15 4.14 3.49 RSD [%] no no yes* no no Outliers CGA 344605 Recovery [%] Recovery Level II - MAL Developing Lab Lab 1 Lab 2 Lab 3 Lab 4 Mean value 100.1 95.2 98.5 98.8 99.5 0.65 0.84 1.70 1.81 0.16 SD 0.65 0.88 1.73 1.83 0.16 RSD [%] yes* no no no no Outliers *Not taken into account all values were calculated 24 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Statistical evaluation Limit of Quantification LOQ A concentration of 0.02 mg/50 mL CGA 344605 was the lowest tested fortification level for which acceptable recovery and precision under repeatability conditions were successfully demonstrated. This concentration is equal to: trifloxystrobin TC trifloxystrobin SC 500 (500 g/L) fluoxastrobin+prothioconazole+trifloxystrobin EC 300 (75+150+75 g/L) trifloxystrobin WG 50 (500 g/kg) 0.040 % (w/w) 0.017 % (w/w) 0.0026 % (w/w) 0.020% (w/w) 25 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Conclusions The statistical evaluation is reported from 5 laboratories which participated in the peer validation. The data presented in the statistical summary show that the method is suitable in terms of accuracy and reproducibility for all samples tested. The acceptance of the proposed method for the determination of the relevant impurity CGA 344605 in trifloxystrobin TC and trifloxystrobin EC, SC and WG formulations tested is recommended. 26 CIPAC 2021, peer validation of rel. impurity CGA 344605 in trifloxistrobin formulations
Thank you. ///////////
