Analytical methods

ExperimentID EXA000630
ChemicalID CH0001638
Chemical Name N,N'-Ethylenebis(dithiocarbamamic acid)
Official Method No
Chromatography LC
Chromatography mfr. ExionLC, AB Sciex
Column RP-Amide 100 mm x 2.1 mm, 3 μm
Column mfr. Ascentis
Detector MS/MS
Detector mfr. QTRAP 6500QT, AB Sciex
Ionization SRM-ESI-negative
Extraction Solvent Extraction
Extraction Details Extracted with Methanol 35 mL, 0.5 % Cysteine / EDTA 40 mL; Shaken vigorously for 15 min. Then, centrifuged 2,000 rpm for 10 min.; Repeated these procedures twice.
Clean-up 1st Column cleanup
Clean-up 1st Details Oasis HLB Plus, 225 mg / 60 μm; Run the extract (after derivatization) through the cartridge at 20 mL / min.; Remove interfering substance with purified water 5 mL; Eluted with Acetonitrile 4 mL
Clean-up 2nd
Clean-up 2nd Details
Clean-up Spike
Syringe Spike
Derivatization Dimethyl sulfate 100 μL; Adjusted to pH7.5-pH8.0 with sodium chloride; Shaken vigorously for 10 min.
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 0.34 ng/g dry
Method Quantification Limit
Repeatability
Standard
Recovery (CRM)
Recovery (spiked)
Recovery (IS)
Protocol https://www.env.go.jp/chemi/kurohon/2021/shosai/5_2_2.pdf
Remarks Analysis method: p.4
RegisterDate 2022/12/08
UpdateDate 2022/12/08