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ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
Chemicals &Reagents
Chemical/Reagent Number/Specification
Appendix A
Reagent/Solution Preparation
Solution Preparation
Monsanto Report Number: MSL0027191 Page 110 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
Standard Calibration and QC Solution Preparation
Overview
Stability
SolutionComponents
SolutionType
Concentrationor Range1,2 Solvent
Approx.Storage
( C)
DemonstratedStability(Days)
DicambaCalibrationStock Solution(0.10 mg/mL)
Monsanto Report Number: MSL0027191 Page 111 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
Dicamba QCStock Solution(0.48 mg/mL)
IntermediateCalibrationSolutions
Intermediate CalibrationSolution (µg/mL) Aliquot Solution ID
AliquotVolume
(mL)
DiluentVolume
(mL)
Monsanto Report Number: MSL0027191 Page 112 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
WorkingCalibrationStandardSolutions
Dicamba Working Calibration Solutions
WorkingCalibration
Solution(µg/mL)
AliquotSolutionConcn
(µg/mL)
AliquotVolume
(mL)
DiluentVolume
(mL)Equivalent Concn1
(ng/PUF)
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.
Monsanto Report Number: MSL0027191 Page 113 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
QCFortificationSolutions
Dicamba QC Fortification Solutions
QC SolutionConcn
(µg/mL) Aliquot Solution ID
AliquotVolume
(mL)
DiluentVolume
(mL)
FortificationConcn
(ng/PUF)
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)
Monsanto Report Number: MSL0027191 Page 114 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
IS WorkingSolution(0.0225 µg/mL)
IS SolutionConcn (µg/mL) Aliquot Solution ID
Aliquot Volume(mL)
ACN Volume(mL)
Sample Preparation Procedure
Sample Storage
SampleProcessing
Step Action
QC Sample Fortification Level (ng/PUF)
Monsanto Report Number: MSL0027191 Page 115 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
Note:
Concentration Factor 25% methanol in water, mL
Monsanto Report Number: MSL0027191 Page 116 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
Injection VolumeAdjustment
Instrumental Analysis
SampleAnalysisGuidance andAcceptanceCriteria
Calibration Curve:
Quality Control Samples:
Monsanto Report Number: MSL0027191 Page 117 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
Injection Carryover:
InstrumentSetup
SystemConditions forAnalysis
LC-MS/MS System Conditions
Monsanto Report Number: MSL0027191 Page 118 of 315
ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS
DataProcessing
Calculations
Overview
Monsanto Report Number: MSL0027191 Page 119 of 315