Analytical methods

ExperimentID EXA000696
ChemicalID CH0000278
Chemical Name Diltiazem
Official Method No
Chromatography HPLC
Chromatography mfr. Prominence UFLC XR, Shimadzu
Column Ascentis Express C18 analytical column (2.7 μm, 100 x 2.1 mm)
Column mfr. Supelco
Detector MS/MS
Detector mfr. AB SCIEX QTRAP 5500 mass spectrometer, Sciex
Ionization ESI
Extraction LLE
Extraction Details Plasma sample (200 μL) was spiked with internal standard solutions, and extracted with a mixture of acetate buffer solution pH 4 (100 μL) and acetonitrile/methanol (1:1 v/v) (600 μL).
Clean-up 1st SPE
Clean-up 1st Details Passed through a HybridSPE-Phospholipid cartridge to remove phospholipids and proteins.
Clean-up 2nd
Clean-up 2nd Details
Clean-up Spike Diltiazem-d3
Syringe Spike
Derivatization
Recovery Correction 97 ± 3.9
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 0.0048 ng/mL
Method Quantification Limit
Repeatability 4.4
Standard
Recovery (CRM)
Recovery (spiked) 110 ± 4.8
Recovery (IS)
Protocol
Remarks Sample: Fish plasma
RegisterDate 2023/1/16
UpdateDate 2023/1/16