Analytical methods

ExperimentID EXA000802
ChemicalID CH0001520
Chemical Name Dicofol
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent; 7890, Agilent
Column DB-5ms 15 m x 0.25 mm
Column mfr. Agilent
Detector HRMS
Detector mfr. AutoSpec Ultima, Waters; AutoSpec Premier, Waters
Ionization SIM-EI
Extraction Solvent Extraction
Extraction Details Extracted with Acetone; Shaken for 10 min., Sonicated for 10 min., then Centrifugated (3,000rpm, 10 min.); Repeated these three times
Clean-up 1st Column cleanup
Clean-up 1st Details Florisil, Anhydrous sodium sulfate; Remove interfering substance with Hexane; Eluted with Dichloromethane/Hexane (50:50)
Clean-up 2nd GPC
Clean-up 2nd Details Gel permeation chromatography: Acetone/Cyclohexane (20:80), Precolumn: Shodex EV-G AC; Column: Shodex EV-2000 AC
Clean-up Spike Dicofol-13C12
Syringe Spike Naphthalene-d8; Acenaphtene-d10; Phenanthrene-d10; Fluoranthene-d10; Chrysene-d12; Decane
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 5 pg/g dry
Method Quantification Limit 13 pg/g dry
Repeatability
Standard
Recovery (CRM)
Recovery (spiked)
Recovery (IS)
Protocol https://www.env.go.jp/chemi/kurohon/2021/shosai/5_3_2.pdf
Remarks Analysis method: p.14
RegisterDate 2023/2/15
UpdateDate 2023/2/15