11 appendices appendix a. analytical method – dicamba … · 11 appendices appendix a. analytical...

11 APPENDICES

Appendix A. Analytical Method – Dicamba on Filter Paper

Monsanto Company Study Number: WBE-2015-0311 Page 21 of 68

Monsanto Report Number: MSL0027193 00 of 308

Monsanto Company Study Number: WBE-2015-0311 2 of 68

Monsanto Report Number: MSL0027193 Page 101 of 308

Appendix B. Analytical Method – Dicamba on Polyurethane Foam

An exact copy of the current version of the analytical method SOP is presented. Thisversion contains the identical methodology used for study sample analysis with minorerror corrections, edits for clarification, formatting updates and additionalwithin-study validation and stability data. A hard copy of the previous SOP version(dated 5/4/2015) is maintained in the study file.



Monsanto Company Method

Effective Date: September 11, 2015 ME-1902-01 Page 1 of 19Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Overview

Purpose &Scope

This document describes the method used by Environmental Sciences TechnologyCenter personnel to determine dicamba on Polyurethane Foam (PUF) air samplingtraps.

MethodSummary

Dicamba is extracted from polyurethane foam (PUF) air sampling traps using methanolcontaining stable-labeled internal standard. The sample tubes are capped and agitatedon a high-speed shaker for extraction. An aliquot of the supernatant is filtered,evaporated, reconstituted in up to 10-fold less volume of 25% methanol in water andthen dicamba is quantitated using LC-MS/MS with electrospray ionization in negativeion mode. The working range of the method is from 0.3 to 75 ng/PUF, with an LOQ of0.3 ng /PUF. Extension of the upper range of the method using lower injectionvolumes was demonstrated during method validation.

SafetyPrecautions

Follow current Monsanto safety policies. Important precautions include:

Some solvents are volatile and/or flammable. Care must be taken to keep themaway from any source of ignition.Ensure proper ventilation to avoid excessive exposure to toxic solvent vapors.Read and follow all safety warnings on reagent containers.Ensure proper safety requirements are followed when operating liquid handlers orautosamplers.

Abbreviations The following abbreviations are used in this method:

Abbreviation DefinitionACS American Chemical SocietyACN acetonitrileamu atomic mass unit

Approx. approximatelyARS Analytical Reference StandardCAD collision assisted dissociationCE collision energy

Concn concentrationCUR curtain gasCXP collision cell exit potentialDP declustering potentialEP entrance potentialESI electrospray ionization

ESTC Environmental Sciences Technology Centerg gram

HPLC high-performance liquid chromatographyIS internal standardL liter

LC-MS/MS liquid chromatography tandem mass spectrometryLOD limit of detectionLOQ limit of quantitation





MeOH methanolmin minutemL millilitermm millimeter

MRM multiple reaction monitoringms millisecondMS mass spectrometryN number of samples

N/A not applicableND not detectedN2 nitrogenng nanogram

PTFE polytetrafluoroethylenePUF polyurethane foam

Q quadrupoleQC quality control

RSD relative standard deviationRT room temperatureµg microgramµl microliter

µm micrometerV volt¨ g relative centrifugal force

Contents Section PageOverview 1Materials 3Reagent/Solution Preparation 4Standard Calibration and QC Solution Preparation 5Sample Preparation Procedure 9Instrumental Analysis 10Calculations 13Documentation 14

AppendicesAppendix A: Compound Structures 15Appendix B: Representative Chromatograms 16Appendix C: Validation Summary 18





Materials

Equipment The following equipment is used in this method. Specific brands are listed to aid theanalyst in finding items. In most cases, equivalent equipment from other vendors maybe used.

Equipment Number/SpecificationAnalytical InstrumentsMass spectrometer AB Sciex API 5000/5500 with Turbo-V

ionization sourceData acquisition system PC workstation with AB Sciex Analyst®

softwareHPLC system Shimadzu Prominence 20A System:

Solvent Degasser, at least 2 Pumps,Autosampler, Heated Column Compartmentand Controller

HPLC switching valve Rheodyne, 6 portHPLC column Phenomenex Kinetex Phenyl-Hexyl

100 mm × 2.10 mm, 2.6 µmSample Preparation EquipmentAnalytical balance Capable of weighing 0.0001 gBottle top dispenser BrandTech Scientific, Cat. No. 4731361Centrifuge Thermo Scientific Sorvall Legend XTRGraduated cylinder (100 mL, 1 L) Suitable for procedureHigh-speed plate shaker SPEX Geno/Grinder® 2010 or comparableLiquid handler Tomtec, Inc. Quadra4 or comparable

pipetting systemMechanical pipettes suitable for procedureRepeating/dispensing pipette Eppendorf Repeater® XstreamSample Preparation ConsumablesPolyurethane Foam (PUF), 22 mmdiameter × 76 mm length

SKC Inc. Cat. No. P22692

Grinding ball, 7/16 inch OPS Diagnostics Cat. No. GBSS 437-1003-03

Polypropylene extraction tubes (50 mL) SARSTEDT Cat. No. 62.548.30496-Well filter plate, 0.2 µm GHP (1 mL) VWR Cat. No. 28148-62496-Well filter plate, 0.2 µm PTFE (2 mL) VWR Cat. No. 89135-71012 mL amber glass sample vials withPTFE lined cap

Fisher Cat. No. 03-391-8D

16 mL amber glass sample vials withPTFE lined cap

Fisher Cat. No. 03-391-8E

96-Well micromat flat bottom Sun-SRI Cat. No. 400-07396-Well square well sealing mat Sun-SRI Cat. No. 401-02696 Deep-well plate, glass coatedpolypropylene (1 mL)

Fisher Cat. No. 60180-P306

96 Deep-well plate, glass coatedpolypropylene (2 mL)

Fisher Cat. No. 60180-P308





Chemicals &Reagents

The following reagents are used in this method. Specific brands are listed to aid theanalyst in finding items. Generally, equivalent reagents and standards obtained fromother vendors may be substituted for the specified product. It is important to use highquality reagents to avoid chromatographic interferences. It is recommended to verifythe isotopic purities of the internal standard materials prior to use.

Chemical/Reagent Number/SpecificationACN, HPLC grade Burdick & Jackson Cat. No. 015-4Water, HPLC grade J.T. Baker Cat. No. 4218-03Methanol, HPLC grade EMD Cat. No. MX0488-1Ethanol, ACS grade Sigma Cat. No. 459844-1LFormic acid, LC-MS grade Sigma Cat. No. 56302-50MLDicamba Monsanto ARS Program(13C6)Dicamba Monsanto ARS Program

(Refer to Appendix A for analyte and internal standard compound structures.)

Reagent/Solution Preparation

Prepare the following reagent solutions for use in sample analysis. The absolutevolume of the solutions may be varied at the discretion of the analyst, as long as thecorrect proportions of the components are maintained. A six-month expiration datewill be assigned to these solutions unless a shorter expiration is specified on the label.Solutions may be stored at room temperature in glass containers, unless otherwisespecified.

Solution PreparationHPLC Mobile Phase A 0.1% formic acid in water: Add 1 mL formic

acid to 1000 mL waterHPLC Mobile Phase B 0.1% formic acid in MeOH: Add 1 mL formic

acid to 1000 mL MeOHHPLC Injection Needle Wash 25% MeOH in water: Add 750 mL water to

250 mL of methanol25% MeOH in water Add 750 mL water to 250 mL of methanol





Standard Calibration and QC Solution Preparation

Overview All standard calibration and fortification solutions must be properly labeled and storedin amber glass vials with airtight lids at approximately 4 C. Preparation procedureswhich result in equivalent solutions may be substituted. Various additional solutionsmay be prepared.

Stability The stability of dicamba in ethanol was demonstrated during the validation of methodME-1321. The stability of dicamba in ACN was demonstrated during the validationof method ME-1381.

SolutionComponents

SolutionType

Concentrationor Range1,2 Solvent

Approx.Storage

( C)

DemonstratedStability(Days)

DicambaStock

Solution100 µg/mL3 Ethanol 4 201

Dicamba

Intermediate and

WorkingCalibrationStandardSolutions

0.010 to 25µg/mL3 ACN 4 201

1 Stability of the stock solutions was established in method ME-1321.2 Stability of intermediate and working solutions was established in method ME-1381.3 Per PR-0897, the stability of dicamba in ethanol is extended to the 0.48 mg/mL QCStock Solution and the stability of dicamba in ACN is extended to 60 µg/mL in theWorking Calibration Solutions.

DicambaCalibrationStock Solution(0.10 mg/mL)

Weigh 10-15 mg (recorded to at least 0.1 mg) of dicamba standard into an aluminumweighing boat. Place weigh boat into an amber glass bottle. Add the appropriatevolume (to the nearest 0.1 mL) of ethanol to prepare a 0.10 mg/mL solution ofdicamba (purity adjusted). An adjustable positive-displacement mechanical pipettecapable of delivering up to 50 mL is recommended. The solution should be sonicatedbriefly to ensure complete dissolution.

Note: The absolute mass and volume of the solutions may be varied at the discretion ofthe analyst, as long as the correct proportions of the components are maintained.





Dicamba QCStock Solution(0.48 mg/mL)

Weigh 10-15 mg (recorded to at least 0.1 mg) of dicamba standard into an aluminumweighing boat. Place weigh boat into an amber glass bottle. Add the appropriatevolume (to the nearest 0.1 mL) of ethanol to prepare a 0.48 mg/mL solution ofdicamba (purity adjusted). An adjustable positive-displacement mechanical pipettecapable of delivering up to 50 mL is recommended. The solution should be sonicatedbriefly to ensure complete dissolution.


IntermediateCalibrationSolutions

Prepare the following intermediate standards by dilution of the appropriate stocksolution in amber glass vials with ACN. These solutions will be used for thepreparation of working calibration standard solutions.

Intermediate CalibrationSolution (µg/mL) Aliquot Solution ID

AliquotVolume

(mL)

DiluentVolume

(mL)

10.0Dicamba Calibration Stock

Solution (0.10 mg/mL)2.50 22.5

1.010.0 g/mL Intermediate

Calibration Solution1.00 9.00

0.11.0 g/mL Intermediate

Calibration Solution1.00 9.00





WorkingCalibrationStandardSolutions

Solutions may be prepared in the following manner. Other concentrations may beused as long as the preparation is documented. A suggested scheme for workingcalibration solution preparation is shown below. For each solution, add the listedaliquot of the designated solution to an amber glass vial and dilute with the specifiedvolume of ACN. Additional solution levels may be prepared as necessary.

Dicamba Working Calibration Solutions

WorkingCalibration

Solution(µg/mL)

AliquotSolutionConcn

(µg/mL)

AliquotVolume

(mL)

DiluentVolume

(mL)Equivalent Concn1

(ng/PUF)0.0015 0.1 0.15 9.85 0.150.00225 0.1 0.225 9.775 0.225

0.003 0.1 0.3 9.7 0.30.0075 0.1 0.75 9.25 0.750.015 1 0.15 9.85 1.5

0.0225 1 0.225 9.775 2.250.03 1 0.3 9.7 30.075 1 0.75 9.25 7.5

0.15 1 1.5 8.5 15

0.225 10 0.225 9.775 22.50.3 10 0.3 9.7 300.75 10 0.75 9.25 75

1 This concentration represents 0.100 mL of Working Calibration Solution diluted bythe extraction solvent (30 fold). For example, 0.100 mL of the 0.015 µg/mL WorkingCalibration Solution diluted to 30 mL results in an equivalent concentration of 1.5 ngdicamba/PUF.





QCFortificationSolutions

Solutions may be prepared in the following manner. Other concentrations may beused as long as the preparation is documented. A suggested scheme for QCfortification solution preparation is shown below. For each fortification solution, addthe listed aliquot of the designated solution to an amber glass vial and dilute with thespecified volume of ACN. Additional fortification solution levels may be prepared asnecessary.

Dicamba QC Fortification Solutions

QC SolutionConcn

(µg/mL) Aliquot Solution ID

AliquotVolume

(mL)

DiluentVolume

(mL)

FortificationConcn

(ng/PUF)1

3.0Dicamba QC Stock Solution

480 µg/mL Dicamba0.15 23.85 NA

0.303.0 µg/mL Dicamba QC

Solution1.0 9.0 NA


Solution0.1 9.9

0.30(LOQ QC)


Solution1.0 9.0

3.00(Mid QC)


Solution2.0 8.0

60(High QC)

6.00Dicamba QC Stock Solution

480 µg/mL Dicamba0.125 9.875

600(Dilution QC)

1 Concentration represents 0.100 mL of QC Fortification Solution diluted by theextraction solvent. For example, 0.100 mL of the 0.030 µg/mL QC Solution diluted to30 mL resulted in an equivalent concentration of 3.0 ng dicamba/PUF.

(13C6)DicambaIS StockSolution(0.10 mg/mL)

Weigh 4-4.5 mg (recorded to at least 0.1 mg) of (13C6)Dicamba standard into analuminum weighing boat. Place weigh boat into an amber glass bottle. Add theappropriate volume (to the nearest 0.1 mL) of ethanol to prepare a 0.10 mg/mLsolution of (13C6)Dicamba. An adjustable positive-displacement mechanical pipettecapable of delivering up to 50 mL is recommended. The solution must be sonicatedbriefly to ensure complete dissolution.






IS WorkingSolution(0.0225 µg/mL)

Solutions may be prepared in the following manner. A suggested scheme for ISsolution preparation is shown below. For each IS solution, add the listed aliquot ofthe designated solution to an amber glass vial and dilute with the specified volume ofACN.

IS SolutionConcn (µg/mL) Aliquot Solution ID

Aliquot Volume(mL)

ACN Volume(mL)

10.0(13C6)Dicamba IS StockSolution (0.10 mg/mL)

1.0 9.0

0.022510.0 µg/mL Dicamba IS

Solution0.225 99.775

Sample Preparation Procedure

Sample Storage Samples will be maintained frozen at approximately -20 °C for extended storageperiods.

SampleProcessing

The following describes the preparation of samples for dicamba analysis by LC-MS/MS. A typical analytical set will include study samples, QCs and standards.

Step Action1 Add a single PUF to each tube designated as a QC.2 Add 0.100 mL of the following solution to the designated sample type:

ACN to test samples and controlsWorking Calibration Solution to calibration standardsQC Fortification Solution to QC samples (e.g. LOQ QC, Mid QC, HighQC and/or dilution QC)QC Sample Fortification Level (ng/PUF)

LOQ QC 0.30Mid QC 3.0High QC 60

Dilution QC 600

3 Add 0.100 mL of the IS Working Solution (0.0225 µg/mL) to all tubes(including tubes designated as standards) using an automated liquid handler orother repeat pipetting device.

4 Add one grinding ball to each tube.5 Add approximately 29.8 mL of MeOH to all tubes using a bottle-top dispenser

or other repeat pipetting device.6 Place a cap on each tube. Ensure the cap is sealed well before proceeding.7 Shake samples on the Geno/Grinder® to extract analyte from the PUF (e.g.,

1200 cycles per minute for 30 minutes). Examine the tubes for leaks. If leaksare detected, discard and re-prepare.

8 Remove cap and transfer 1.8 mL of supernate to clean 96-well filter plate (2mL) with a clean glass-lined polypropylene plate (2 mL) positioned below thefilter plate.

9 Pass the samples through the filter plate.





10 Discard the filter plate. Evaporate the samples to dryness under nitrogen.Note: This step is performed at 50 °C. Typical setting: N2 = 40 L/min.

11 Add appropriate volume of 25% methanol in water solution. Up to a 10xconcentration factor was demonstrated during method validation. Exampleconcentration factors given in table below.

Concentration Factor 25% methanol in water, mL10 x 0.1805 x 0.3602 x 0.9001 x 1.80

Note: This concentration procedure maintains the response ratio in thesamples; therefore, it is not necessary to enter a dilution factor in thecalculations.

12 Cover the 96-well plate with a micromat flat bottom cap mat. Ensure the capmat is sealed well before proceeding.

13 Mix well and analyze by LC-MS/MS within the storage time determined duringmethod validation.





Injection VolumeAdjustment

High-level samples producing an analyte response greater than that of the higheststandard of the calibration curve must be re-injected with a smaller injection volume(down to 5 µL) so the analyte response of the sample is within the analyte responserange of the standards. This procedure maintains the response ratio. It is notnecessary to enter a dilution factor in the calculations. Note: The response ratio maynot be within the range of response ratios of the standards. A “dilution QC” must beincluded and pass acceptance criteria to accept small injection volume data. The re-injected sample may be analyzed in any chromatographic set.

If multiple injections of a study sample are performed, the first acceptable result willbe reported.

Instrumental Analysis

SampleAnalysisGuidance andAcceptanceCriteria

Acceptance criteria for study samples utilizing this analytical method are:

Calibration Curve:

Calculated calibration standard concentrations used to determine results must be

Calibration points may be removed for a documented analytical reason or a

removed and not included in the calculation, provided they do not change theestablished regression model (e.g., linear 1/x weighting). If a calibrationstandard(s) is removed the reason must be documented in the raw data (i.e.,inaccuracy >20%).A minimum of six concentration levels (excluding blanks) and at least 75% of thetotal number of calibration standards must be represented in the final curve.

Quality Control Samples:

The acceptance criterion for QC fortifications is a mean accuracy range of 70-

RSD at each fortification level.A maximum of 1 outlier (i.e., falls outside of acceptance criteria or fails Grubbsoutlier test) may be discarded at each QC fortification level. Proper justificationand documentation of discarded outliers must be performed.Any response in QC control samples falling within the retention window of a

where this response is exceeded, the presence of the target analyte (i.e.,inadvertent contamination) in representative samples versus an unknowninterference will be assessed using an appropriate confirmatory technique. Theresults will be assessed by the Study Director.Each batch run must contain a minimum of duplicate QC control samples andtriplicate fortifications at the LOQ and at least one higher QC level.In addition, for in-study validation purposes, at least one of the control sampleswill be run with a minimum of 5 replicate fortifications at the LOQ and at leastone higher level.





If low volume injection is needed, then capability of low volume injection will bedemonstrated by including dilution QC samples in the study. The dilution QCsamples must meet the same acceptance criteria for accuracy and precision forquality control samples as stated above.

Injection Carryover:

The potential for carryover will be evaluated in each analytical or batch run byplacing a double blank after the highest calibration curve point.

the LOQ level.

InstrumentSetup

Instrument operation is controlled by acquisition methods containing all autosampler,HPLC, switching valve, source interface and mass spectrometer parameters.Precursor and product ions for the analytes are shown below along with choices forpossible use in confirmatory analyses. Alternate ions may be used for quantitation orconfirmation if they provide better data (sensitivity and/or specificity). The use of aminimum of one quantitation transition and one confirmatory transition is required foreach batch run. The transitions used for these purposes will be clearly designated.The following equipment and conditions are instrument/system dependent and may bemodified to obtain optimal instrument performance and maximize sensitivity.Injection volume may be modified to extend the dynamic range of the method. Actualmethod parameters must be documented in the raw data.

SystemConditions forAnalysis

LC-MS/MS System Conditions

HPLC: Shimadzu Prominence 20AMass spectrometer: AB Sciex API 5000/5500Ion source: Turbo-VColumn: Phenomenex Kinetex Phenyl-Hexyl Column, 100 mm × 2.10 mm, 2.6 µmInjection volume: 50 µLAutosampler temperature: 4 °CColumn oven temperature: 50 °CMobile Phase A: water with 0.1% formic acidMobile Phase B: MeOH with 0.1% formic acidHPLC Gradient Conditions:

Time (min) %BTotal Flow(mL/min) Divert

0 25 0.3 To MS0.5 25 0.3 To MS1.0 50 0.3 To MS4.0 61 0.3 To MS4.1 95 0.3 To MS5.5 95 0.3 To waste5.6 95 0.6 To waste10.9 95 0.6 To waste11.0 25 0.6 To waste11.5 25 0.6 To waste11.6 25 0.3 To waste





15.0 Controller StopRun time: 15 min (MS data collection 5.5 min)

Mass Spectrometer ConditionsMode: negative ionScan type: MRMResolution Q1: unitResolution Q3: unitProbe type: ESIDuration : 5.5 minCurtain gas (CUR): 10Collision gas (CAD): 2Gas 1: 50 N2

Gas 2: 50 N2

IonSpray voltage (IS): -2000 VInterface heater: onTemperature (TEM): 450 °CScan time (ms): 250

Analyte:Precursor

Ion Q1(amu)

ProductIon Q3(amu)

DP(V)

EP(V)

CE(V)

CXP(V)

Dicamba 219 175 -45 -10 -10 -10(13C6)Dicamba(IS)

225 181 -45 -10 -10 -10

Confirmatory IonsDicamba 221 177 -45 -10 -10 -10(13C6)Dicamba(IS)

227 183 -45 -10 -10 -10

DataProcessing

Process the data using the Analyst® quantitation wizard. The wizard is used to processthe data for the MRM transition pairs established in the acquisition method. Themethod detects and integrates the analyte peaks based on retention time and MRMtransition. Chromatograms may be smoothed prior to integration as long as thesmoothing is consistent throughout the entire chromatographic set. Manual peakintegration should be used when the automated procedure is not effective due tobaseline noise. Dilution factors, if applicable, must be added during data processing ifnot input prior to the start of the instrument run.

Calculations

Overview Analyte concentrations are calculated using the Analyst® software. The softwarecalculates the standard curve and applies the dilution factor to account for dilution orconcentration during processing. Standard curves are generated as the ratio of theanalyte response (e.g., peak area) to the internal standard response, for each standardlevel, plotted against concentration (i.e., ratio of analyte concentration to internalstandard concentration). A linear regression model is used for quantitation with orwithout weighting (e.g. linear 1/x weighted). All the samples from a study must beanalyzed with the same type of calibration curve (i.e., plot axes and weighting) for agiven analyte transition.





AnalyteConcentration

Analyte concentrations are reported as ng/PUF. The Analyst® software automaticallycalculates the raw concentration of the injected sample relative to the standard curve(calculated concentration). This value is also automatically multiplied by any valueentered in the dilution factor column.

Assumptions:1) The nominal dilution of the sample during extraction (1:30) is incorporated into the

calibration standard concentrations that are entered into the Analyst® software.The calibration standard concentrations are entered as equivalent concentrations(‘Equivalent Concn (ng/PUF)’ in the Working Calibration Solution tables above).Calibration standard solutions are diluted equivalently to samples in the sampleprocessing procedure of the method; therefore, these entered concentrations are 30times their actual injected concentrations, so the dilution factor is eliminated.

2) Entry of a dilution factor is not required for samples using a reduced injectionvolume or extract concentration (the original analyte/IS response ratio ismaintained).

Documentation

The analytical raw data packages will include (at a minimum): the sample processingworksheet (form(s)), instrumental sample queue/run record, calibration curves, MRMchromatograms, results tables, and instrument acquisition parameters.

Example Chromatograms

Example chromatograms for calibration standards, control samples and fortifiedsamples are provided in Appendix B.

Method Validation Results

Method Validation Summary is provided in Appendix C.

Superseded method(s): N/AAuthor(s): Leah S. Riter





Appendices

Appendix A: Compound Structures

Ý´

Ý´ Ñ

ÝØí

Ñ ÑØ Dicamba

3,6-dichloro-2-methoxybenzoic acidCAS # 1918-00-9

C8H6Cl2O3

Average Molecular weight: 221.04

ïíÝ

ïíÝïíÝ

ïíÝ

ïíÝ

ïíÝ

Ý´

Ý´ Ñ

ÝØí

Ñ ÑØ (13C6)Dicamba

3,6-dichloro-2-methoxybenzoic-1,2,3,4,5,6-13C6 acidCAS #1173023-06-7

C213C6H4Cl2O3

Average Molecular weight: 227.04



Effective Date: September 11, 2015Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC

Appendix B: Representative Chromatograms

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September 11, 2015 ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC

Chromatograms

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Dicamba 1

Dicamba 2

Page 16 of 19Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

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Dicamba 1

Dicamba 2



Effective Date: September 11, 2015Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC

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Dicamba 1: untreated control (left); IS (right)Dicamba 2: fortified control 0.3 ng/PUFDicamba 3: calibration standard 0.3


September 11, 2015 ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC

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Dicamba 1: untreated control (left); IS (right)g/PUF, ppm (left); IS (right)

ng/PUF, ppm (left); IS (right)

Dicamba 3

Page 17 of 19Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

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Dicamba 3



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