Propiconazole + Chlorothalonil
Section 13:
Formulation:
To be Determined
EPA Reg. No:
To be Determined
CAS No.:
Propiconazole: 60207-90-1;
Registrant:
Syngenta
Chlorothalonil: 1897-45-6
Section 27: (Special note for chlorothalonil only in large font)
Store samples in a limited access area at temperatures that will maintain frozen sample integrity (generally less
than -20C), until extraction.
The samples may be stored whole or ground, depending on the standard procedure of the analytical laboratory.
However, if maceration will cause residue deterioration, then samples must be stored whole until analysis.
For Chlorothalonil Only:
Since maceration of the samples may cause residue deterioration:
All treated samples must be stored whole until shortly before (2 – 3 days) extraction.
It is preferred that the untreated samples be stored whole until shortly before (2 – 3
days) extraction however, if needed (for method development, validation, storage
stability set-up, etc., a few of the untreated samples may be ground/processed
earlier and the processed samples must be stored frozen until extraction.
For all Analytes:
Continue with rest of Sec. 27 of protocol.
Section 28:
Reference Substance(s): Propiconazole and 2,4-Dichlorobenzoic Acid (2,4-DCBA), and the triazole metabolites
1,2,4-Triazole (T), Triazole Alanine (TA) and Triazole Acetic Acid (TAA) and/or chlorothalonil (R044686 or SDS-2787)
and it’s metaolite 4-hydroxy-2,5,6-trichloroisophthalonitrile (R182281 or SDS-3701)
(Add to end of paragraph): Internal standards and derivatized standards may also be needed depending on the
method used. These may also be obtained by contacting the registrant.
Registrant for RS only if different than Section 13:
NA
Section 29:
REFERENCE METHODS:
For Propiconazole:
1. Total Propiconazole Method:
"Determination of Total Residues of Propiconazole in Crops as 2,4-Dichlorobenzoic Acid Methyl Ester by
Capillary Gas Chromatography," Analytical Method No. AG-626, Novartis Crop Protection, Inc., October 10,
1997.
AND
2. Parent Propiconazole Only Method:
Syngenta Analytical Method REM 130.11, "Residue Analytical Method for the Determination of Residues of
Propiconazole (CGA64250) in Crop Samples. Final Determination by LC-LC-MS/MS.", T. Clark, 12/1/05.
AND
3. Triazole Metabolite Method:
"Determination of 1,2,4-Triazole, Triazole Alanine and Triazole Acetic Acid Residues in Plant and Animal
Matrices," Analytical Method No. Meth-160, Revision #2, Morse Laboratories, LLC, Sacramento, CA, 95825,
April 13, 2005.
For Chlorothalonil:
R044686 - Analytical Method for the Determination of Total Chlorothalonil Residues in Crop Commodities by LCMS/MS. Heubner, M.R., June 25, 2010; Syngenta Analytical Method GRM005.03A.
OR
Syngenta Method GRM005.01A “Chlorothalonil (R44686): Analytical Method for the Determination of Residues
of Chlorothalonil and R182281 in Crops” Author: S. Chaggar; Dated: 31 October 2006.
REFERENCE METHOD MODIFICATIONS/METHOD VALIDATION:
For Propiconazole:
For Total Propiconazole Method (1): To validate the method (1), fortify some of the control samples in
triplicate with propiconazole at a minimum of 3 concentration levels, lowest level of method validation (0.05 ppm
or lower), 0.5 ppm, and 5 ppm.
A minimum of 6 fortification samples (recovery spikes) for each crop fraction, at the lowest level of method
validation (LLMV) is required prior to completion of the analytical phase of the study. The acceptable recovery
range is 70-120%. Documented approval from the Study Director is needed for recoveries outside of this
range.
For Propiconazole Parent Only Method (2): To validate the methods (2), fortify some of the control samples
in triplicate with propiconazole at a minimum of 3 concentration levels, lowest level of method validation (0.01
ppm or lower), 0.5 ppm, and 5 ppm.
A minimum of 6 fortification samples (recovery spikes) for each crop fraction, at the lowest level of method
validation (LLMV) is required prior to completion of the analytical phase of the study. The acceptable recovery
range is 70-120%. Documented approval from the Study Director is needed for recoveries outside of this
range.
For 1,2,4-Triazole, (T), Triazole Alanine (TA) and Triazole Acetic Acid (TAA): To validate the method (3),
fortify some of the control samples in triplicate with propiconazole at a minimum of 3 concentration levels each,
lowest level of method validation (0.01 ppm or lower), 0.1 ppm, and 1 ppm.
A minimum of 6 fortification samples (recovery spikes) for each crop fraction, at the lowest level of method
validation (LLMV) is required for each analyte prior to completion of the analytical phase of the study. The
acceptable recovery range is 70-120%. Documented approval from the Study Director is needed for
recoveries outside of this range.
For Chlorothalonil:
To validate the method, fortify some of the control samples in triplicate with chlorothalonil and SDS 3701 at a
minimum of 3 concentration levels each, lowest level of method validation (0.01 ppm or lower for chlorothalonil,
and SDS 3701), 0.3 and 5 ppm.
A minimum of 6 fortification samples (recovery spikes) for each crop fraction, at the lowest level of method
validation (LLMV) is required prior to completion of the analytical phase of the study. The acceptable recovery
range is 70-120%. Documented approval from the Study Director is needed for recoveries outside of this
range.
SAMPLE ANALYSIS:
For Propiconazole:
Samples will be analyzed for residues of propiconazole (using both methods 1 & 2) and the triazole metabolites
T, TA and TAA (using method 3) following the Working Methods. For each field trial associated with this study,
analyze at least one untreated and all treated residue samples for each matrix.
For Chlorothalonil:
Samples will be analyzed for the residues of chlorothalonil and R182281 following the Working Method. For
each field trial associated with this study, analyze at least one untreated and all treated residue samples for each
matrix.
STORAGE STABILITY ANALYSIS:
As soon as possible after receipt of samples, a minimum of six subsamples of all available crop fractions of the
control shall be fortified with Propiconazole at 0.5 ppm, and the triazole metabolites 1,2,4-Triazole (T), Triazole
Alanine (TA) and Triazole Acetic Acid (TAA) at 0.1 ppm each, and/or Chlorothalonil (R044686 or SDS-2787) and
R182281 at 0.3 ppm.
Use this language if adequate SS data is available or SS data is not needed:
Please contact the Study Director to determine if storage stability samples need to be analyzed.
Only if directed by the Study Director, …..
Special instructions if needed may be added (with notes) at the end of each sub-section.