Table S1 Clinical bioanalysis summary information for study A
Test compound
Fostamatinib disodium
Analytical matrices
Plasma (K2-EDTA)
Urine
Semen
Analytes
R406
R406 N-glucuronide
R788
Internal standard (IS)
R940406-d9
[2-H, 13-C] R788
Validated methods
R406 plasma
R788 plasma
R406 urine
R406 N-glucuronide urine
R406 semen
Lower limit of quantification
R406 plasma: 0.250 ng/mL
R788 plasma: 0.500 ng/mL
R406 urine: 1.000 ng/mL
R406 N-glucuronide urine: 10.000 ng/mL
R406 semen: 0.250 ng/mL
Validated range
R406 plasma: 0.250–250 ng/mL
R788 plasma: 0.500–250 ng/mL
R406 urine: 1.000–1000 ng/mL
R406 N-glucuronide urine: 10.000–5000 ng/mL
R406 semen: 0.250–250 ng/mL
Quality control (QC) levels
R406 plasma: 0.750, 25.000, 200, 5000 (dilution QC) ng/mL
R788 plasma: 1.50, 25.000, 200 ng/mL
R406 urine: 3.000, 100, 800 ng/mL
R406 N-glucuronide urine: 30, 500, 4000, 50,000 (dilution QC)
ng/mL
1
R406 semen: 0.750, 25.000, 200 ng/mL
Analytical technique/method of detection
R406 plasma: Liquid-liquid extraction, LC-MS/MS
R788 plasma: Protein precipitation, LC-MS/MS
R406 urine: Liquid-liquid extraction, LC-MS/MS
R406 N-glucuronide urine: Dilution with methanol, LC-MS/MS
R406 semen: Liquid-liquid extraction, LC-MS/MS
Total number of samples analyzed
R406 plasma: 1658
R788 plasma: 586
R406 urine: 312
R406 N-glucuronide urine: 312
R406 semen: 6
Sample storage conditions
In a freezer set to maintain approximately –70°C (–60 to –80°C)
LC-MS/MS liquid chromatography coupled with tandem mass spectrometry
2
3