Copper pyrithione - Europadissemination.echa.europa.eu/Biocides/ActiveSubstances/... ·...
Transcript of Copper pyrithione - Europadissemination.echa.europa.eu/Biocides/ActiveSubstances/... ·...
Competent Authority Report According to Directive 98/8/EC
Copper pyrithione CAS 14915-37-8
Active substance in Biocidal Products
Product Type 21 (Antifouling products)
Applicant: Arch Chemicals Inc.
DOCUMENT III A Section 4: Analytical Methods for Identification and Detection
Rapporteur Member State: Sweden
Final CAR September 2014
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Table of Contents; DOC III-A Section 4
Section A.4 Analytical Methods for Detection and Identification ........................................................ 3
Section A4.1/01 Determination of the pure active substance and impurities in the technical material ...... 3
Section A4.1/02 Determination of the pure active substance and impurities in the technical material ...... 6
Section A4.1/03 Determination of the pure active substance and impurities in the technical material ...... 7
Section A4.2(a)/01 Determination of residues in soil .................................................................................... 11
Section A4.2(b)/01 Determination of residues in air ...................................................................................... 16
Section A4.2(b)/02 Determination of residues in air ...................................................................................... 19
Section A4.2(c)/01 Determination of residues in water (fresh water) ............................................................ 24
Section A4.2(c)/02 Determination of residues in water (drinking) ................................................................ 28
Section A4.2(c)/03 Determination of residues in water (seawater) ................................................................ 32
Section A4.2(d)/01 Determination of residues in animal and human body fluids and tissues (plasma) ........ 36
Section A4.2(d)/02 Determination of residues in animal and human body fluids and tissues ...................... 41
Section A4.3/01 Determination of residues in/on food or feedstuffs ......................................................... 43
Reference list of studies submitted by Section No. ............................................................................................... 48
Reference list of studies submitted by Author ...................................................................................................... 49
Al'ch Chemicals Inc .. RMS: Sweden
Section A.4
Section A4.1/01
Annex Point IIA, IV.4.1
1.1 Reference
1.2 Data pl'otection
1.2. l Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2.1 Guideline study
2.2 GLP
2.3 Deviations
3.1 Pl'eliminal'y tl'eatment
3.1.1 Enriclunent
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard
3.2.4 Interfering substance
3.3 Lineal"ity
3.3.1 Calibration range
3.3.2 Number of
Coppel' pyrithione Septembel' 2014
Analytical Methods for Detection and Identification
Determination of the pure active substance and impur ities in the technical material
Active substance
1. REFERENCE
Document IV ARCPT 4010-001
Final CAR Doc III A4
Official use only
•••• (2006) Copper Pyrithione - 5 Batch characterisation, ITS Testing Services (UK) Ltd. Study Number 1298506 (unpublished)
• -2. GUIDELINES AND QUALITY ASSURANCE
OPPTS 830.1700
Yes
None
3. MATERIALS AND METHODS
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Section A4.1/01
Annex Point IIA, IV.4.1
mea.sm·ements
3.3.3 Linearity
3.4 Specifity: interfering substances
3.5 Recovel'y rates at diffel'ent levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Pl'ecision
3.7.1 Repeatability
Coppel' pyrithione August 2013
Determination of the pure active substance and impurities in the technical material
Active substance
3.7.2 Independent -laboratory validation
4.1 M aterials and methods
4.2 Conclusion
4.2.1 Reliability
4.2.2 Deficiencies
4. APPLICANT'S SUMMARY AND CO NCLUSION
The method may be used to assay TGAI copper pyrithione
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Date
Materials and methods
Conclusion
Reliability
Acceptability
Rema1·ks
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Determination of the pure active substance and impurities in the technical material
Active substance
Evaluation by Competent Authorities
EVALUATION BY RAPPORTEUR MEMBER STATE
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RMS: Sweden
Copper pyrithione
September 2014
Final CAR
Doc III A4
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Section A4.1/02 Determination of the pure active substance and
impurities in the technical material
Annex Point IIA, IV.4.1 Impurities
The validation data for the analysis of impurities in the technical copper
pyrithione is confidential information and is presented in the Annex
Confidential Data and Information
Al'ch Chemicals Inc .. RMS: Sweden
Section A4.1/03
Annex Point IIA, IV.4.1
1.1 Refel'ence
1.2 Data pl'otection
1.2. l Data owner
1.2.2 Companies with letter of access
1.2.3 Criteria for data protection
2.1 Guideline study
2.2 GLP
2.3 Deviations
3.1 Pl'eliminal'y tl'eatment
3.1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard
3.2.4 Interfering substance
3.3 Linea1·ity
3.3.l Calibration range
3.3.2 Number of measurements
Coppel' pyrithione Septembel' 2014
Final CAR Doc IIIA4
Determination of the pure active substance and impurities in the technical material
Assay of TGAI in AF fol'mulations
1. REFERENCE
Document IV ARCPT 4011-003
- (2003) Validation of analytical method: HPLC detemiination of copper pyrithione in marine antifouling paints, Arch Cheniicals, Inc. Cheshire, CT, Repo1t No. CASR-03-2003 (m1published) --2. GUIDELINES AND QUALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3. MATERIALS AND METHODS
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3.3.3 Linearity
3.4 Specifity: intel'fering substances
3.5 Recovel'y rates at diffel'ent levels
3.5.1 Relative standard deviation
3.6 Limit of detel'mination
3.7 Pl'ecision
3.7.1 Repeatability
3.7.2 Independent
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Determination of the pure active substance and impurities in the technical material
Assay of TGAI in AF fol'mulations
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4.1 Materials and methods
4.2 Conclusion
4.2.l Reliability
4.2.2 Deficiencies
Date
Materials and methods
Conclusion
Reliability
Coppel' pyrithione August 2013
Determination of the pure active substance and impurities in the technical material
Assay of TGAI in AF fol'mulations
4. APPLICANT'S SUMMARY AND CONCLUSION
[CONFIDENTIAL INFORMATION EXCLUDED] .
CAR DocIIIA4
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The method may be used for analysis of copper pyrithione in paint in the range of0.5% - 7.5%.
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EVALUATION BY RAPPORTEUR MEMBER STATE
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Annex Point IIA, IV.4.1
Ac.ceptability
Rema1·ks
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Determination of the pure active substance and impurities in the technical material
Assay of TGAI in AF fol'mulations
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Section A4.2(a)/01
Annex Point IIA, IV.4.2(a)
1.1 Refel'ence
Determination of residues in soil
1 REFERENCE
Document IV ARCPT 4020-001
••• (2004) Method for the analysis of pyrithione in sediment by HPLC with MS/MS detection. Arch Chemicals, Inc. Cheshire, CT, USA, Report No. CASR-01-2004 (unpublished)
1.2 Data pl'otec.tion •
1.2.1 Data owner
1.2.2 Companies with letter -of access
1.2.3 Criteria for data protection
2.1 Guideline study
2.2 GLP
2.3 Deviations
3.1 Pl'eliminal'y ti·eatment
3 .1.1 Enrichment
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
2 GUIDELINES AND QUALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3 MATERIALS AND METHODS
-
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Official use only
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Section A4.2(a)/01 Determination of residues in soil
Annex Point IIA, IV.4.2(a) Zinc pyrithione
3.2.3 Standard( s)
3.2.4 Interfering substance( s)
3.3 Linea1·ity
3.3.l Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specifity: interfering substances
3.5 Recovery rates at diffel'ent levels
3.5. l Relative standard deviation
3.6 Limit of determination
3. 7 Pl'ecision
3. 7 .1 Repeatability
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4 APPLICANT 'S SUMMARY AND CONCLUSION
4.1 M aterials and methods
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4.2 Conclusion
4.2. l Reliability
4.2.2 Deficiencies
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Determination of residues in soil
The method was validated with sediment, but also applies to analysis of pyrithione in soils since the matrix is similar and variations in extraction efficiency are compensated for by the intemal standard.
Pyrithione fonns strong complexes with various metal ions (e.g., zinc, copper, and iron) and may also complex with metallic or other cationic sites in the sediment. Although the concentration of pyrithione in sediment or soil may be expressed for convenience as the e.quivalent concentration of it is impo1tant to understand that at low concentrations in sediment (and the similar mati·ix, soil) do not exist as a single compounds. This may be deduced from the general chemistry of chelation compounds. As discussed in the section on fate and behavior in water, experimental data exist that show in water readily trnnschelates to copper pyrithione in the presence of copper(II). Soil and sediment are much more complex matrices, containing a variety of charged sites and various metal ions at concentrations much higher those predicted for pyrithione. Evidence that both compounds dissociate and interact with the sediment to fonn a. common set of pyrithione complexes was obta.ined from aquatic metabolism studies conducted with which showed that both compounds degraded at the same rate and the degradation products exhibited the same pattem of formation and decline.
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EVALUATION BY RAPPORTEUR MEMBER STATE
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Annex Point IIA, IV.4.2(a)
Date
Materials and methods
Conclusion
Reliability
Acceptability
Rema1·ks
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Determination of residues in soil
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Table A4.2(a)/01: Charactel'istics of the sediment (loamy-sand) used in the validation (Rittel', 2004)
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Section A4.2(b )/01
Annex Point IIA, IV.4.2(b)
1.1 Refer ence
Copper pyrithione September 2014
Determination of residues in air
1. REFERENCE
Document IV ARCPT 4020-002
- (2001) Analysis of on sample collection media in suppo1t of an application occupational exposure study. Arch Chemicals, Inc., Study Number 73-00B lOCuPT (unpublished)
1.2 Data protection •
1.2 . l Data owner
1.2 .2 Companies with letter -of access
1.2 .3 Criteria for data protection
2.1 Guideline study
2.2 GLP
2.3 Deviations
3.1 P1·elhnina1-y treatment
3 .1.1 Extraction
3 .1.2 Cleanup
3.2 Detection
3.2 . l Separation method
2. GUIDELINES AND QUALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3. MATERIALS AND METHODS
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Section A4.2(b )/01 Determination of residues in air
Annex Point IIA, IV.4.2(b) Copper p y1ithlone
3.2.2 Dete.ctor
3.2.3 Standard( s)
3.2.4 Interfering substance(s)
3.3 Linea1ity
3.3.1 Calibration range
3.3.2 Nwnber of I measurements
3.3.3 Linearity
3.4 Specificity : intedering substances
3.5 Recove1·y 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 -labora.to1y validation
4.1 Materials and methods
4. APPLICANT'S SUMMARY AND CONCLUSION
[CONFIDENTIAL Il'i"FORMATION EXCLUDED] .
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Annex Point IIA, IV.4.2(b) Copper py1ithlone
4.2 Conclusion
4.2. l Reliability
4.2.2 Deficiencies
Date
Materials and methods
Conclusion
Reliability
Ac.ceptability
Rema1·ks
The method is applicable for quantitation of copper pyrithione in the range of0.5 µg to 200 µg collected on the sampling filters.
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EVALUATION BY RAPPORTEUR MEMBER STATE
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Annex Point IIA, IV.4.2(b)
1.1 Reference
1.2
1.2.1
1.2.2
1.2.3
2.1
2.2
2.3
Data pl'otection
Data ov.111er
Companies with letter of access
Criteria for data protection
Guideline study
GLP
Deviations
3.1 Pl'eliminal'y tl'eatment
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CAR Doc III A4
Determination of residues in air
1 REFERENCE
Document IV EZPTF 4020-006
• (2007) Analytical method validation for the determination of
•••• in air sampling collection media, Arch Chemicals, Inc., Cheshire, CT, USA, Identification No. CASR-05-2007 (unpublished) .
• -2 GUIDELINES AND QUALITY ASSURANCE
Not applicable
Yes
No
3 MATERIALS AND METHODS
Official use only
3.1.1 Enrichment -
3.1.2 Cleanup -
3.2 Detection
3.2.1 Separntion method
3.2.2 Detector
3.2.3 Standard(s)
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Section A4.2(b )/02
Annex Point IIA, IV.4.2(b)
3.2.4 Interfering substance( s)
3.3 Lineal'ity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specificity: intel'fering substances
3.5 Recovel'y rates at diffel'ent levels
3.5.1 Relative standard deviation
3.6 Limit of detel'mination
3.7 Pl'ecision
3.7.1 Repeatability
3.7.2 Independent laborato1y validation
4.1 M atel'ials and methods
4.2 Conclusion
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Determination of residues in air
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-4 APPLICANT 'S SUMMARY AND CONCLUSION
This method is suitable for measurement of······ concentrations in air using air sampling filters. The limit of quantitation is 0.2 µg colle.cted on the filter. The con-esponding air concentration depends on the volume of air sampled. No breakthrough occtmed at a flow rate of 1.5 Uminute for 5 hours, con-esponding to
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4.2.1 Reliability
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CAR Doc IIIA4
Determination of residues in air
450 liters sampled. The LOD in air is therefore at least 0.44 µg/m3.
The instmmentation required to perfonn the analysis is available in most well equipped analytical laboratories. No toxic or hazardous reagents are required to prepare the samples, and all of the sample preparation equipment is commercially available. The method does not require the use of tmtreated commodity to coITect for recoveries.
The method uses - as the external calibration standard, but the derivative reacts with the pyrithione portion of the molecule. The method is therefore applicable to measmement ofNaPT and CuPT as well as ZnPT. Results expressed as ZnPT concentration can be converted to CuPT or NaPT concentrations by applying the appropriate molecular weight ratio.
NaPT concentrntion = - concentration) x (2) x (149.15) I (317 .67)
CuPT concentrntion = ~concentration) x (315.86) I (317 .67)
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EVALUATION BY RAPPORTEUR MEMBER STATE
Date
Materials and methods
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Annex Point IIA, IV.4.2(b)
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Determination of residues in air
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Section A4.2(b )/02
Annex Point IIA, IV.4.2(b)
Conc.lusion
Reliability
Ac.ceptability
Rema1·ks
Coppel' pyrithione August 2013
Determination of residues in air
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Section A4.2(c)/01
Annex Point IIA, IV.4.2(c)
1.1 Reference
1.2 Data protection
1.2 .1 Data owner
1.2 .2 Companies with letter of access
1.2 .3 Criteria for data protection
2.1 Guideline study
2.2 GLP
2.3 Deviations
3.1 P1·elimina1-y treatment
3.1.l Extraction
3.1.2 Cleanup
3.2 Detection
3.2.1 Separation method
Copper pyrithione September 2014
Determination of residues in water (fresh water)
1. REFERENCE
Document IV ARCPT 4020-003
••••••• (2003) Detemlination of copper pyrithione in freshwater by high performance liquid chromatography. Method validation at 0.1 µg/L concentrntion. Arch Chemicals, Inc. Cheshire, CT, USA, Report No. CASR-02-2003 (unpublished)
-2. GUIDELINES AND QUALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3. MATERIALS AND METHODS
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3.2 .2 Detector
3.2 .3 Standard( s)
3.2.4 Interfering substance( s)
3.3 Linea1ity
3.3. 1 Calibration range
3.3.2 Nwnber of measurements
3.3.3 Linearity
3.4 Specificity: intel"fering substances
3.5 Recovery rntes at differ ent levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7. l Repeatability
3.7.2 Independent laboratory validation
4.1 Materials and methods
4.2 Conclusion
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Determination of residues in water (fresh water)
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-4. APPLICANT'S SUMMARY AND CONCLUSION
[CONFIDENTIAL INFORMATION EXCLUDED] .
This method is suitable for use by regulato1y agencies to detect pyrithione in SW'face and drinking water. The instrumentation required to perform the analysis is available in most well equipped analytical laboratories. No toxic or hazardous reagents are required to prepare the samples, and all of the sample preparation equipment is commercially available. The method does not require the use of untreated commodity to correct for recoveries.
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Determination of residues in water (fresh water)
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Evaluation by Competent Authorities
Date
Matel'ials and methods
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Conc.lusion
Reliability
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Annex Point IIA, IV.4.2(c)
Acceptability
Remal'ks
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Determination of residues in water (fresh water)
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Section A4.2(c)/02
Annex Point IIA, IV.4.2
1.1 Refe1·ence
1.2
1.2. l
1.2.2
1.2.3
2.1
2.2
2.3
Data pl'otection
Data owner
Companies with letter of access
Criteria for data protection
Guideline study
GLP
Deviations
3.1 Pl'eliminal'y treatment
Coppel' pyrithione August 2013
CAR Doc IIIA4
Determination of residues in water (drinking)
1 REFERENCE
Document IV ARCPT 4020-003
••• (2007) Method for the analysis of copper pyrithione in drinking water by HPLC with MS/MS detection. Arch Chemicals, Inc. Cheshire, CT, USA, Report No. CASR-07-2007 (unpublished)
• -2 GUIDELINES AND QUALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3 MATERIALS AND METHODS
Official use only
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3.1.2 Cleanup -
3.2 Detection
3.2.1 Separation method
3.2.2 Detector
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Section A4.2(c)/02
Annex Point IIA, IV.4.2
3.2.3 Standard( s)
3.2.4 Interfering substance( s)
3.3 Linea1·ity
3.3.1 Calibration range
3.3.2 Number of measurements
3.3.3 Linearity
3.4 Specificity: intel'fering substances
3.5 Recovel'y rates at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Pl'ecision
3.7.1 Repeatability
3.7.2 Independent laborato1y validation
4.1 Materials and methods
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Determination of residues in water (drinking)
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• -4 APPLICANT'S SUMMARY AND CONCLUSION
Extenal standards are prepared at concentrations of 0.0498, 0.0996 0.249, 0.996, 2.49, and 9.96 µg/L in HPLC grade water. One milliter of each standard and each water sample a.re derivatized by addition of l 0 ul of a 20-mg/ml solution of the derivatizing reagent •••• ••••••••••••••••••• After a reaction time of20 minutes a.t 65 dgerees C, 60 µL of each are injected onto the HPLC co1Ull11l. The pyrithione derivative elutes with a. retention time of3.9 - 4.0 minutes.
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4.2 Conclusion
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Determination of residues in water (drinking)
CAR Doc IIIA4
A linear least squares analysis of the standards concentration vs. peak area (l /x weighting) is used to calculate the copper py:rithione concentration in the samples.
The method was validated using residential well water. This method is X8 suitable for use by regulatory agencies to detect copper pyrithione in surface and drinking water. The instrumentation required to perfonn the analysis is available in most well equipped analytical laboratories. No toxic or hazardous reagents are required to prepare the samples, and all of the sample preparation equipment is commerciaily available. The method does not require the use of untreated commodity to coffe.ct for recovenes .
4.2.1 Reliability I
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Evaluation by Competent Authorities
Date
Materials and methods
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Conclusion
Reliability
Accep tability
Rema1·ks
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Determination of residues in water (drinking)
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Annex Point IIA, IV.4.2
1.1 Refe1·ence
1.2
1.2. l
1.2.2
1.2.3
2.1
2.2
2.3
Data pl'otection
Data owner
Companies with letter of access
Criteria for data protection
Guideline study
GLP
Deviations
3.1 Pl'eliminal'y tl'eatment
Coppel' pyrithione August 2013
CAR Doc IIIA4
Determination of residues in water (seawater)
1 REFERENCE
Document IV EZPTF 4020-008
••• (2009) Method for the analysis of pyrith.ione in seawater by HPLC with MS/MS detection. Arch Chemicals, Inc. Cheshire, CT, USA, Repo1t No. CASR-02-2009 (unpublished)
• -2 GUIDELINES AND Q UALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3 MATERIALS AND METHODS
Official use only
3 .1.1 Enriclunent -
3.1.2 Cleanup -
3.2 Detection
3.2.1 Separation method X l
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3.2.2 Detector
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3.2.3 Standard(s)
3.2.4 Interfering substance( s)
3.3 Lineal"ity
3.3.1 Calibration range
3.3.2 Number of measw-ements
3.3.3 Linearity
3.4 Specificity: 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
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Determination of residues in water (seawater)
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4.1
laborato1y validation
Materials and methods
4.2 Conclusion
4.2.1 Reliability
4.2.2 Deficiencies
Date
Materials and methods
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Determination of residues in water (seawater)
-4 APPLICANT'S SUMMARY AND CONCLUSION
CAR Doc IIIA4
The method uses intemal standard calibration. Standards are prepared contammg at 5-6 concentration levels in the range of 0.05 to 10 µg/L in HPLC grade water. Three-milliliter aliquots of each standard and sample are spiked with ••••••••••• (intemal standard) at a concentration of 0.4 ug/L and derivatized by addition of 15 µL of a 20-mg/ml solution of the derivatizing reagent ••••••••••••••••••• After a reaction time of20 minutes at 65° C, 50 µL of each are analyzed by HPLC with detection by positive ion electrospray ionization mass spectrometry in the multiple reaction monitoring scan mode. The pyrithione derivative elutes with a retention time of·····
A linear least squares analysis (l/x weighting) of the standard concentration vs. the /IS peak area ratio is used to calculate the concentration in the samples.
The method was validated using sea.water. The instrumentation required to perform the analysis is available in most well equipped analytical laboratories. No toxic or hazardous reagents are required to prepare the samples, and all of the sample preparation equipment is commercially available. The method does not require the use of untreated commodity to cotl'ect for recoveries.
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Evaluation by Competent Authorities
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Section A4.2(c)/03
Annex Point IIA, IV.4.2
Conclusion
Reliability
Accep tability
Rema1·ks
Coppel' pyrithione August 2013
Determination of residues in water (seawater)
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Arch Chemicals Inc .. RMS: Sweden
Section A4.2( d)/01
Annex Point IIA, IV.4.2(d)
1.1 Refer ence
1.2 Data protection
1.2 .l Data owner
1.2 .2 Companies with letter of access
1.2 .3 Criteria for data protection
2.1 Guideline s tudy
2.2 GLP
2.3 Deviations
3.1 Prelimina1·y treatment
3.1.1 Extr action
3.1.2 Cleanup
3.2 Detection
Copper pyrithione September 2014
Final CAR Doc IIIA4
Determination of residues in animal and human body fluids and tissues (plasma)
1. REFERENCE
Document IV E ZPTF 4020-004, EXPTF 4020-005
- (2002) Quantitation of total pyrithione in rat plasma via HPLC with MS/MS detection. PPD Development, Richmond, VA, USA, Method No. LCMSC 2 18 Version 1.00 (llllpublished)
•••• (2003) Validation of a high-perfonnance liquid chromatography/mass spectrometry method for the analysis of total pyrithj ione in rat plasma. PPD Development, Richmond, VA, USA, Validation Report No. LCMSC 218 Version 1.00 (tmpublished)
•
-2. GUIDELINES AND Q UALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3. MATERIALS AND METHODS
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Section A4.2( d)/01
Annex Point IIA, IV.4.2(d)
3.2.1 Separation method
3.2.2 Detector
3.2.3 Standard( s)
3.2.4 Interfering substance(s)
3.3 Linea1ity
3.3. 1 Calibration range
3.3.2 Nmuber of measmements
3.3.3 Linearity
3.4 Specificity: intel'fel'ing substances
Coppel' pyrithione August 2013
Determination of residues in animal and human body fluids and tissues (plasma)
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Section A4.2( d)/01
Annex Point IIA, IV.4.2(d)
3.5 Recove1·y rntes at different levels
3.5.1 Relative standard deviation
3.6 Limit of determination
3.7 Precision
3.7.l Repeatability
Copper pyrithione August 2013
CAR Doc III A4
Determination of residues in animal and human body fluids and tissues (plasma)
XS
•
- - - - -- - - - - ----• •
3.7.2 Independent -laboratory validation
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Annex Point IIA, IV.4.2(d)
4.1 Matel'ials and methods
4.2 Conclusion
4 .2 . l Reliability
4.2 .2 Deficiencies
Date
Matel'ials and methods
Coppel' pyrithione August 2013
CAR Doc IIIA4
Determination of residues in animal and human body fluids and tissues (plasma)
4. APPLICANT 'S SUMMARY AND CONCLUSION
[CONFIDENTIAL INFORMATION EXCLUDED] .
This method is suitable for use by regulatory agencies to detect X6 pyrithione in blood plasma and in principle may be adapted for analysis in other body fluids and tissues. Stable label is used as the internal standard; however, the actual analyte a.ft.er derivatization is the uncomplexed pyrithione molecule, which is the form that both -•••••••••••• takes in biological fluids. The method is therefore applicable to copper pyrithione as well. The instnunenta.tion required to perfo1m the analysis is available in most well equipped analytical laboratories.
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Section A4.2( d)/01
Annex Point IIA, IV.4.2(d)
Conc.lusion
Reliability
Ac.ceptability
Remai-ks
Coppel' pyrithione August 2013
Determination of residues in animal and human body fluids and tissues (plasma)
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Section A4.2( d)/02
Annex Point IIA, IV.4.2(d)
Detailed justification:
Date
Evaluation of applicant 's justification
Conclusion
Rema1·ks
Coppel' pyrithione Septembel' 2014
Determination of residues in animal and human body fluids and tissues
Final CAR Doc IIIA4
JUSTIFICATION FOR NON-SUBMISSION OF DATA Official use only
XI
Evaluation by Competent Authorities
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Arch Chemicals Inc.
RMS: Sweden
Copper pyrithione
August 2013
CAR
Doc III A4
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Section A4.3/01
Annex Point IIIA, IV.1.
Detailed justification:
Date
Evaluation of applicant's justification
Conc.lusion
Rema1·ks
Coppel' pyrithione Septembel' 2014
Determination of residues in/on food or feedstuffs
Final CAR DocIIIA4
JUSTIFICATION FOR NON-SUBMISSION OF DATA Official use only
Evaluation by Competent Authorities
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Section A4.3/01
Annex Point IIIA, IV.1.
1.1 Reference
1.2
1.2.1
1.2.2
1.2.3
2.1
2.2
2.3
3.1
3.1.l
3.1.2
3.2
3.2.l
Data protection
Data ovmer
Companies with letter of access
Criteria for data
protection
Guideline study
GLP
Deviations
Preliminary
treatment
Enriclunent
Cleanup
Detection
Separation method
3.2.2 Detector
Copper pyrithione August 2013
CAR Doc III A4
Analytical Methods for Detection and Identification
Environmental Media - Residues in Fish and Shellfish
1 REFERENCE
••• (2009) Method for the Analysis of Pyrithione in Fish Muscle by HPLC with MS/MS Detection, Arch Chemicals, Inc. Cheshire, CT, Report No. CASR-02-2008 (unpublished) .
• -2 GUIDELINES AND QUALITY ASSURANCE
Not applicable
Not applicable
Not applicable
3 MATERIALS AND METHODS
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Annex Point IIIA, IV.1.
3.2.3 Standard(s)
3.2.4 Interfering substance( s)
3.3 Linea1·ity
3.3.1 Calibration range
3.3.2 Number of
measlll'ements
3.3.3 Linearity
3.4 Specificity:
intel'fering substances
3.5 Recovel'y rates at differ ent levels
3.5.1 Relative standard
deviation
3.6 Limit of
determination
3.7 Pl'ecision
3.7.1 Repeatability
3.7.2 Independent laborato1y validation
Coppel' pyrithione August 2013
Analytical Methods for Detection and Identification
Environmental Media - Residues in Fish and Shellfish
•
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Section A4.3/01
Annex Point IIIA, IV.1.
4.1 Materials and methods
4.2 Conclusion
4.2. l Reliability
4.2.2 Deficiencies
Date
Materials and methods
Copper pyrithione August 2013
Analytical Methods for Detection and Identification
Environmental Media - Residues in Fish and Shellfish
4 APPLICANT'S SUMMARY AND CONCLUSION
The method is accuarate and specific for pyrithione in fish at
concentrations equivalent to 0.5 to 5 ng/Kg of either copper or •
I None
Evaluation by Competent Authorities
EVALUATION BY RAPPORTEUR MEMBER STATE
46 (49)
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Section A4.3/01
Annex Point IIIA, IV.1.
Condusion
Reliability
Ac.ceptability
Rema I' ks
Coppel' pyrithione August 2013
Analytical Methods for Detection and Identification
Environmental Media - Residues in Fish and Shellfish
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47 (49)
CAR Doc IIIA4
Arch Chemicals Inc.
RMS: Sweden
Copper pyrithione
August 2013
CAR
Doc III A4
48 (49)
Reference list of studies submitted by Section No.
See document I
Arch Chemicals Inc.
RMS: Sweden
Copper pyrithione
September 2014
Final CAR
Doc III A4
49 (49)
Reference list of studies submitted by Author
See document I