June 25, 2018
Assay System:
- Human liver microsomes (HLM), pooled from 50 donors.
- Incubation of the test compound with HLM in the presence of NADPH with collection of samples from the incubation mixture at 6 time points.
- The remaining activity of individual CYP enzymes measured using isoform-specific probe substrates with LC/MS/MS detection to determine the rate constant of CYP inactivation (kobs). The experiment is repeated at 6 concentrations of the test compound to measure the dependence of kobs on inactivator concentration.
- Constants KI (equilibrium binding) and kin (irreversible CYP inactivation) for test compounds are determined from the kinetic data using a non-linear regression analysis to the four-parameter logistic model fit with XLFit 5.3 from IDBS software.
Assay Conditions:
Test Compound Concentration | Six concentrations ranging around values of IC50 shift (determined from time-dependent inhibition experiments) |
Microsome Concentration | 0.1 mg/mL |
Percent Organic Solvent in Incubation | 2% acetonitrile |
CYP Isoforms Available for Testing | CYP1A2, CYP2C9, CYP2C19, CYP2D6, and CYP3A4 |
Pre-Incubation Time | 30 minutes |
Incubation Time | up to 30 minutes (depending on CYP isoform) |
pH | 7.4 |
Temperature | 37°C |
Analysis | LC-MS/MS |
Number of Repeats | 2 |
Deliverable: Values of KI (µM), kinact(min-1), and kinact/KI (mL/min/µmol) for test compounds and positive control inhibitors
Test Compound Requirement: 1-2 mg dry powder or 100-200 µL of 10 mM acetonitrile stock solution.
CYP Isoform | Probe Substrate | Monitored Metabolite | Positive Control Inhibitor |
1A2 | Phenacetin | Acetaminophen | Furafylline |
2C9 | Tolbutamide | 4’-OH Tolbutamide | Tienilic Acid |
2C19 | S-Mephenytoin | 4’-OH Mephenytoin | (S)-Fluoxetine |
2D6 | Dextromethorphan | Dextrorphan | Paroxetine |
3A4 | Testosterone | 6β-OH Testosterone | Mibefradil |
3A4 | Midazolam | 1’-OH Midazolam | Mibefradil |