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Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 1 of 3
Section A4.1 (01)
Annex Point IIA4.1
Analytical methods for the determination of pure active substance
and, where appropriate, for relevant degradation products, isomers
and impurities of the active substance and additives (e.g. stabilisers)
TI-435 technical grade active ingredient (TGAI)
1 REFERENCE Official
use only
1.1 Reference Kramer, H.T., Telleen, K. (2001): Analytical method for analysis of
TI-435 technical grade active ingredient (TGAI).
Covance, Harrogate, England; unpublished part of report no. 6155-119
1.2 Data protection Yes
1.2.1 Data owner Sumitomo Chemical Takeda Agro Co., Ltd.
1.2.2 Companies with
letter of access
None
1.2.3 Criteria for data
protection
Data on existing a.s. submitted for the first time for entry into Annex I.
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study Yes
OPPTS 830.1800
2.2 GLP No
2.3 Deviations No
3 MATERIALS AND METHODS
3.1 Preliminary
treatment
3.1.1 Enrichment No enrichment performed. The sample is diluted in methanol and
directly injected on the HPLC.
3.1.2 Cleanup No clean-up performed. The sample is diluted in methanol and directly
injected on the HPLC.
3.2 Detection
3.2.1 Separation method Liquid chromatography (HPLC) using reversed phase conditions
3.2.2 Detector UV detector, wavelength: 265 nm
3.2.3 Standard(s) Internal standard: 3-nitrophenol
3.2.4 Interfering
substance(s)
None for the conditions applied in this study.
3.3 Linearity
3.3.1 Calibration range 53.7 µg/mL to 202 µg/mL
3.3.2 Number of
measurements
Duplicate injections for each of the three standard concentrations
3.3.3 Linearity Correlation coefficient r2 = 1
3.4 Specificity:
interfering
substances
The specificity of the method was demonstrated by examining the
chromatographic peaks of the active ingredient for peak purity by
HPLC-UV DAD. The peak purity indicated that no interferences were
found.
3.5 Recovery rates at
different levels
Five samples of one batch were fortified with known amounts of TI-435
reference substance (ratio 1:1) and analysed. The recoveries ranged
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 2 of 3
Section A4.1 (01)
Annex Point IIA4.1
Analytical methods for the determination of pure active substance
and, where appropriate, for relevant degradation products, isomers
and impurities of the active substance and additives (e.g. stabilisers)
TI-435 technical grade active ingredient (TGAI)
from 98.7% to 101.7% and the mean recovery was 100.4% ( 1.13%).
3.5.1 Relative standard
deviation
1.1%
3.6 Limit of
determination
Not determined. It deemed unnecessary for TI-435 technical materials
whose purity is more than 95%.
3.7 Precision
3.7.1 Repeatability Five analysis of one batch were performed on each of two different days
(10 analysis in total). The relative standard deviations were 0.9% on the
first day, 1.7% on the second day and overall, the relative standard
deviation was 1.3%.
3.7.2 Independent
laboratory
validation
Not relevant
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and
methods
An analytical method for the analysis of TI-435
was validated according to OPPTS 830.1800. TI-435
was diluted in methanol and analysed directly by liquid chromatography
(HPLC) using reversed phase conditions and UV detection.
Linearity, specificity, accuracy (recovery rates) and repeatability of the
analytical method were determined.
4.2 Conclusion Validity criteria of the analytical method presented can be considered as
fulfilled. Linearity, specificity, accuracy and repeatability of the
analytical method have been demonstrated.
4.2.1 Reliability
4.2.2 Deficiencies
Evaluation by Competent Authorities
Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date 08.11.04
Materials and methods
The applicant´s version is acceptable.
Conclusion Applicant´s version is adopted.
Reliability 2
Acceptability acceptable
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 3 of 3
Section A4.1 (01)
Annex Point IIA4.1
Analytical methods for the determination of pure active substance
and, where appropriate, for relevant degradation products, isomers
and impurities of the active substance and additives (e.g. stabilisers)
TI-435 technical grade active ingredient (TGAI)
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers
and to applicant´s summary and conclusion.
Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
Remarks
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 1 of 2
Section A4.1/02
Annex Point IIA4.1
Analytical methods for the determination of pure active substance
and, where appropriate, for relevant degradation products, isomers
and impurities of the active substance and additives (e.g. stabilisers)
TI-435 technical grade active ingredient (TGAI) and impurities
1 REFERENCE Official
use only
1.1 Reference Kramer, H.T., Telleen, K. (2001b): Preliminary analysis of TI-435
technical grade active ingredient (TGAI).
Covance, Harrogate, England; unpublished revised report no. 6155-119,
January 10, 2001, amended on January 15, 2002 and January 17, 2003
1.2 Data protection Yes
1.2.1 Data owner
1.2.2 Companies with
letter of access
1.2.3 Criteria for data
protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study Yes
US EPA OPPTS 830.1700
2.2 GLP Yes
2.3 Deviations None
3 MATERIALS AND METHODS
The identity and analysis of TI-435 technical grade active ingredient and
impurities are confidential information.
4 APPLICANT'S SUMMARY AND CONCLUSION
The identity and analysis of TI-435 technical grade active ingredient and
impurities are confidential information.
4.1 Conclusion Validity criteria of the analytical method can be considered as fulfilled.
4.1.1 Reliability 1
4.1.2 Deficiencies No
Evaluation by Competent Authorities
Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date 21.10.04
Materials and methods
The applicant’s version is acceptable.
Conclusion Applicant´s version is adopted
Reliability 1
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 2 of 2
Section A4.1/02
Annex Point IIA4.1
Analytical methods for the determination of pure active substance
and, where appropriate, for relevant degradation products, isomers
and impurities of the active substance and additives (e.g. stabilisers)
TI-435 technical grade active ingredient (TGAI) and impurities
Acceptability acceptable
Remarks Please find the information in the confidential part of the CA-report: Confidential
data and information; Doc. III; Doc. III-A; III-A_02_01_cloth
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers
and to applicant´s summary and conclusion.
Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
Remarks
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 1 of 4
Section A4.2 (01) Annex Point IIA4.2
Analytical methods including recovery rates and the
limits of determination for the active substance, and for
residues thereof, and where relevant in/on the following:
(a) Soil
1 REFERENCE
Official
use only
1.1 Reference Schramel, O. (2000): Residue analytical method 00540 (MR-654/98) for
determination of TI-435 and the metabolites TZNG and MNG in soil by
Liquid Chromatography with electrospray MS/MS-detection.
Bayer AG, unpublished report no. MR-654/98
1.2 Data protection Yes
1.2.1 Data owner Sumitomo Chemical Takeda Agro Co., Ltd. and Bayer CropScience
1.2.2 Companies with
letter of access
None
1.2.3 Criteria for data
protection
Data on existing a.s. submitted for the first time for entry into Annex I.
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study No
2.2 GLP Yes
2.3 Deviations Not relevant
3 MATERIALS AND METHODS
3.1 Preliminary
treatment
3.1.1 Enrichment Mixing of 20 g of soil with 4 g hydromatrix
Transfer of soil/hydromatrix-mixture into a stainless steel cartridge of
an ASE extractor
Extraction at 80°C with approx. 50 mL acetonitrile/ water/ acetic acid
(200 : 800 : 0.8, v/v/v) for 5 min.
Addition of 1 ml internal standard (d3 -TI-435, 13
C,15
N- TZNG, and
d3 -MNG)
Adjustment to 50 mL with acetonitrile/ water (1:4, v/v)
3.1.2 Cleanup No purification of the soil extract was performed.
3.2 Detection
3.2.1 Separation method HPLC
3.2.2 Detector Electrospray MS/MS-detection in the Multiple Reaction Monitoring
mode
3.2.3 Standard(s) Isotopically labelled internal standard (d3 -TI-435, 13
C,15
N- TZNG, and
d3 -MNG) to compensate for possible matrix effects in the MS/MS
detector
3.2.4 Interfering
substance(s)
None
3.3 Linearity
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 2 of 4
Section A4.2 (01) Annex Point IIA4.2
Analytical methods including recovery rates and the
limits of determination for the active substance, and for
residues thereof, and where relevant in/on the following:
(a) Soil
3.3.1 Calibration range TI-435: 1.07 - 534.1 µg/L
TZNG: 1.11 - 494.8 µg/L
MNG: 1.07 - 533.5 µg/L
3.3.2 Number of
measurements
9 levels measured
3.3.3 Linearity TI-435: R² = 0.9999
TZNG: R² = 0.9997
MNG: R² = 0.9995
3.4 Specifity:
interfering
substances
Since the HPLC MS/MS determination is highly specific, a
confirmatory method is not required. This was confirmed by well
resolved peaks which were obtained at both fortification levels.
3.5 Recovery rates at
different levels
The method was validated in two different soils:
1. BBA 2.2: weak loamy sand/loamy sand*, pH (CaCl2): 6.3,
CEC: 10 meq/100 g, 4.3% org. matter, 7.2% clay
2. Hoefchen: heavy loamy silt/silty loam*, pH (CaCl2): 6.7,
CEC: 13 meq/100 g, 1.6% org. matter, 19% clay
* classifications according to DIN / USDA
Soil samples were fortified at and above the limit of quantitation
(0.005 mg/kg and 0.05 mg/kg) prior to the extraction procedure. The
recoveries are detailed in Table A4_2_01-1.
3.5.1 Relative standard
deviation
3.6 Limit of
determination
Control samples were amended with a standard solution of TI-435,
TZNG and MNG to achieve fortification levels of 0.005 mg/kg and
0.05 mg/kg. The lowest fortification level experimentally tested at
which acceptable recovery data have been obtained was 0.005 mg/kg for
TI-435 and its metabolites. Accordingly, this level corresponds (per
definition) to the limit of quantitation (LOQ).
LOQ = 0.005 mg/kg TI-435, TZNG and MNG
The limit of detection was 0.002 mg/kg for TI-435 and its metabolites.
3.7 Precision
3.7.1 Repeatability The repeatability was determined by 10 measurements of the standard
solution of 0.1 mg/L. The intensity ratios of TI-435 to d3 -TI-435,
TZNG to 13
C,15
N-TZNG and MNG to d3 -MNG were determined. The
relative standard deviations of the intensity rations were 2.5% for TI-
435, 2.9% for TZNG and 2.1% for MNG.
3.7.2 Independent
laboratory
validation
Not relevant
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 3 of 4
Section A4.2 (01) Annex Point IIA4.2
Analytical methods including recovery rates and the
limits of determination for the active substance, and for
residues thereof, and where relevant in/on the following:
(a) Soil
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and
methods
A method for the residue analysis of TI-435
was presented and validated. After extraction of
fortified soil samples, TI-435 in the soil extracts were
analysed directly by HPLC with Electrospray MS/MS-detection.
d3 -TI-435, 13
C,15
N- TZNG, and
d3 –MNG)
Linearity, specificity, recovery rates, limit of determination and
quantitation (LOD and LOQ) and repeatability of the analytical method
were determined.
4.2 Conclusion The analytical method presented permits the determination of residues
of TI-435 in soil with satisfactory
accuracy and precision. Therefore, the method is considered valid for
the determination of residues of TI-435 in soil.
4.2.1 Reliability 1
4.2.2 Deficiencies No
Evaluation by Competent Authorities
Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date 2004-12-02
Materials and methods
Applicant's version is adopted with exception of points 3.4 Specifity and 4.2.2
Deficiencies. A confirmation of positive results without a second analytical
method is possible only, if at least two product ions were monitored with LC-
MS/MS.
Conclusion The method is considered valid for the determination of residues of TI-435,
TZNG and MNG in soil as primary method.
Reliability 1
Acceptability acceptable
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers
and to applicant´s summary and conclusion.
Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
Remarks
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 4 of 4
Table A4_2_01-1: Recovery in %
Fortification level 0.005 mg/kg wet soil 0.05 mg/kg wet soil
n mean range rel. SD mean range rel. SD overall
TI-435
BBA 2.2 5 108 103-112 3.5 100 95 -104 3.1
Hoefchen 5 103 97 -111 5.3 101 96 -107 4.6
mean : 103
rel. SD : 4.9
TZNG
BBA 2.2 5 99 85 -112 10.6 104 95 -109 5.2
Hoefchen 5 96 85 -106 10.1 101 94 -109 5.3
mean : 100
rel. SD : 7.9
MNG
BBA 2.2 5 107 100-112 4.4 94 92 - 96 2.2
Hoefchen 5 101 91 -110 7.2 94 87 - 99 5.2
mean : 99
rel. SD : 7.3
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.2 (02) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
1 REFERENCE Officialuse only
1.1 Reference (2001):
1.2 Data protection Yes
1.2.1 Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study No
2.2 GLP Yes
2.3 Deviations Not relevant
3 MATERIALS AND METHODS
3.1 Preliminary treatment
3.1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard(s)
3.2.4 Interfering substance(s)
3.3 Linearity
RCC project no. 852224 Page 1 of 3
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.2 (02) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specifity: interfering substances
3.5 Recovery rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.1 Repeatability
3.7.2 Independent laboratory validation
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and methods
A method for the residue analysis of TI-435 in soil was presented and validated. After extraction of fortified soil samples, TI-435 in soil extracts were analysed directly by HPLC with UV detection.
Linearity, specificity, recovery rates, limit of determination and quantitation (LOD and LOQ) and repeatability of the analytical method were determined.
A second HPLC column of different polarity was used for confirmation analysis.
4.2 Conclusion The analytical method presented permits the determination of residues of TI-435 in soil with satisfactory accuracy and precision. Therefore, the method is considered valid for the determination of residues of TI-435 in soil.
4.2.1 Reliability 1
4.2.2 Deficiencies No
RCC project no. 852224 Page 2 of 3
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 3 of 3
Section A4.2 (02) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
Evaluation by Competent Authorities Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
Conclusion
Reliability
Acceptability
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers and to applicant´s summary and conclusion. Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
Remarks
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 April 2005
Section A4.2 (03) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
1 REFERENCE Officialuse only
1.1 Reference (1999):
1.2 Data protection
1.2.1 Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study No
2.2 GLP Yes
2.3 Deviations Not relevant
3 MATERIALS AND METHODS
3.1 Preliminary treatment
3.1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard(s)
3.2.4 Interfering substance(s)
RCC project no. 852224 Page 1 of 5
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 April 2005
Section A4.2 (03) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
3.3 Linearity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specifity: interfering substances
3.5 Recovery rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.1 Repeatability
3.7.2 Independent laboratory
RCC project no. 852224 Page 2 of 5
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 April 2005
Section A4.2 (03) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
validation
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and methods
A method for the residue analysis of TI-435 in soil was presented and validated. After
extraction of fortified soil samples, TI-435, in the soil extracts were analysed directly by HPLC with
Electrospray MS/MS-detection.
Linearity, specificity, recovery rates, limit of determination and quantitation (LOD and LOQ) and repeatability of the analytical method were determined.
4.2 Conclusion The analytical method presented permits the determination of residues of TI-435 in soil with satisfactory accuracy and precision. Therefore, the method is considered valid for the determination of residues of TI-435,
in soil.
4.2.1 Reliability 1
4.2.2 Deficiencies No
Evaluation by Competent Authorities Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
Conclusion
Reliability
Acceptability
Remarks
COMMENTS FROM ...
Date
Results and discussion
Conclusion
Reliability
Acceptability
RCC project no. 852224 Page 3 of 5
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 April 2005
Section A4.2 (03) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(a) Soil
Remarks
RCC project no. 852224 Page 4 of 5
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 April 2005
RCC project no. 852224 Page 5 of 5
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.2 (04) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(b) Air
1 REFERENCE
Officialuse only
1.1 Reference (2000):
1.2 Data protection
1.2.1 Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study Yes Commission Directive 96/46EC of July 16, 1996 Directive 91/414/EEC – guideline on residue analytical method Document 8064/VI/97 rev. 4 (15/12/1998)
2.2 GLP Yes
2.3 Deviations No
3 MATERIALS AND METHODS
3.1 Preliminary treatment
3.1.1 Sampling
3.1.2 Enrichment
3.1.3 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard(s)
3.2.4 Interfering substance(s)
3.3 Linearity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
RCC project no. 852224 Page 1 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.2 (04) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(b) Air
3.4 Specifity: interfering substances
3.5 Recovery rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.1 Repeatability
3.7.2 Independent laboratory validation
RCC project no. 852224 Page 2 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.2 (04) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(b) Air
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and methods
A method for residue analysis of TI-435 in air was described and validated. The required limit of quantification was defined based on toxicological parameters . Approximately 1/10 and a 5-fold of this concentration were analysed. The method is based on the guidance documents Commission Directive 96/46EC and Directive 91/414/EEC – guideline on residue analytical method Document 8064/VI/97 rev. 4 (15/12/1998).
Linearity, specificity, recovery rates, limit of determination and quantification (LOD and LOQ) and repeatability of the analytical method were determined.
4.2 Conclusion The analytical method presented permits the determination of residues of TI-435 in air with satisfactory accuracy and precision. Therefore, the method is considered valid for the determination of residues of TI-435 in air. The results obtained by the confirmatory method (HPLC-UV using a CN phase) were in good agreement with the results obtained by the HPLC-UV method using a reversed phase.
4.2.1 Reliability 1
4.2.2 Deficiencies No
Evaluation by Competent Authorities Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
Conclusion
Reliability
Acceptability
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers and to applicant´s summary and conclusion. Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
RCC project no. 852224 Page 3 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 4 of 4
Section A4.2 (04) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(b) Air
Remarks
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 1 of 3
Section A4.2 (05) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(c) Water
1 REFERENCE
Official use only
1.1 Reference (2000):
1.2 Data protection
1.2.1 Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study SANCO/825/00 rev. 6 of 20/06/00 of the European Commission
2.2 GLP Yes
2.3 Deviations No
3 MATERIALS AND METHODS
3.1 Preliminary treatment
3.1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard(s)
3.2.4 Interfering substance(s)
3.3 Linearity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specifity: interfering substances
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 2 of 3
Section A4.2 (05) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(c) Water
3.5 Recovery rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.1 Repeatability
3.7.2 Independent laboratory validation
3.8 Confirmation analysis
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and methods
A method for residue analysis of TI-435 in drinking and surface water was presented and validated.
-435 was analysed directly by HPLC with UV detection. The method is based on guidance document SANCO/825/00 rev. 6 of 20/06/00 of the European Commission.
Linearity, specificity, recovery rates, limit of determination and quantification (LOD and LOQ) and repeatability of the analytical method were determined.
4.2 Conclusion The analytical method presented permits the determination of residues of TI-435 in drinking and surface water with satisfactory accuracy and precision. Therefore, the method is considered valid for the determination of residues of TI-435 in drinking and surface water.
4.2.1 Reliability 1
4.2.2 Deficiencies No
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 3 of 3
Section A4.2 (05) Annex Point IIA4.2
Analytical methods including recovery rates and the limits of determination for the active substance, and for residues thereof, and where relevant in/on the following:
(c) Water
Evaluation by Competent Authorities
Use separate "evaluation boxes" to provide transparency as to the comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
Conclusion
Reliability
Acceptability
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers and to applicant´s summary and conclusion. Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
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Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.3/01 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
1 REFERENCE
Officialuse only
1.1 Reference (2000c):
1.2 Data protection
1.2.1 Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study Yes SANCO/825/00 rev. 6 of 20/06/00 of the European Commission and BBA Guideline: Residue Analytical Methods for Post-Registration Control Purposes of July 21, 1998
2.2 GLP Yes
2.3 Deviations No
3 MATERIALS AND METHODS
3.1 Preliminary treatment
3.1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Column
3.2.4 Standard(s)
3.2.5 Interfering substance(s)
RCC project no. 852224 Page 1 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.3/01 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
3.3 Linearity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specifity: interfering substances
3.5 Recovery rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.1 Repeatability
3.7.2 Independent laboratory validation
3.8 Confirmation analysis
RCC project no. 852224 Page 2 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.3/01 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and methods
A method for the determination of the residue of TI-435 in plant material is presented and validated. Specimens of apple, wheat, sugar-beet and oil seed rape were extracted with acetone / water .
the samples were analysed by HPLC. The method is based on SANCO/825/00 rev. 6 of 20/06/00 of the European Commission. Linearity, specificity, recovery rates, limit of determination and quantitation (LOD and LOQ) and repeatability of the analytical method were determined.
4.2 Conclusion The analytical method presented permits the determination of residues of TI-435 in tested matrices with satisfactory accuracy and precision. Therefore, the method is considered valid for the determination of residues of TI-435 in plant material.
4.2.1 Reliability 1
4.2.2 Deficiencies No
Evaluation by Competent Authorities Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
Conclusion
Reliability
Acceptability
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers and to applicant´s summary and conclusion. Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
RCC project no. 852224 Page 3 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 4 of 4
Section A4.3/01 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.3/02 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
1 REFERENCE
Officialuse only
1.1 Reference (2001):
1.2 Data protection
1.2.1 Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2 GUIDELINES AND QUALITY ASSURANCE
2.1 Guideline study Yes SANCO/825/00 rev. 6 of 20/06/00 of the European Commission and BBA Guideline: Residue Analytical Methods for Post-Registration Control Purposes of July 21, 1998
2.2 GLP Yes
2.3 Deviations No
3 MATERIALS AND METHODS
3.1 Preliminary treatment
3.1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
RCC project no. 852224 Page 1 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.3/02 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
3.2.3 Column
3.2.4 Standard(s)
3.2.5 Interfering substance(s)
3.3 Linearity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specifity: interfering substances
3.5 Recovery rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.1 Repeatability
3.7.2 Independent laboratory validation
3.8 Confirmation analysis
RCC project no. 852224 Page 2 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
Section A4.3/02 Annex Point IIIA IV.1
Analytical methods including recovery rates and the limits of determination for residues in/on food or feedstuffs and other products where relevant
4 APPLICANT'S SUMMARY AND CONCLUSION
4.1 Materials and methods
An analytical method is presented that describes the additional validation of method
for determination of the active substance in plant material. The method is based on SANCO/825/00 rev. 6 of 20/06/00 of the European Commission. Linearity, specificity, recovery rates, limit of determination and quantitation (LOD and LOQ) and repeatability of the analytical method were determined.
4.2 Conclusion The analytical method presented permits the determination of residues of TI-435 in tested matrices with satisfactory accuracy and precision down to a limit of quantitation of Therefore, the method is considered valid for the determination of residues of TI-435 in plant material.
4.2.1 Reliability 1
4.2.2 Deficiencies No
Evaluation by Competent Authorities Use separate "evaluation boxes" to provide transparency as to the
comments and views submitted
EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
Conclusion
Reliability
Acceptability
Remarks
COMMENTS FROM ...
Date Give date of comments submitted
Results and discussion Discuss additional relevant discrepancies referring to the (sub)heading numbers and to applicant´s summary and conclusion. Discuss if deviating from view of rapporteur member state
Conclusion Discuss if deviating from view of rapporteur member state
Reliability Discuss if deviating from view of rapporteur member state
Acceptability Discuss if deviating from view of rapporteur member state
Remarks
RCC project no. 852224 Page 3 of 4
Sumitomo Chemical Takeda Agro Co., Ltd. TI-435 February 2004
RCC project no. 852224 Page 4 of 4