Table I Summary of fractionation and LC-MS drug assay conditions
DrugFractionation conditionsLC-MS systemLC drug assay conditionsTransition monitoredIonization modeInjection volume
MTXMethod 1Agilent 1200 binary HPLC TSQ Quantum Access triple quadrupoleC18 (400 μl min−1)455.0 → 307.6Positive ESI100 μl
RadicicolMethod 1Agilent 1200 binary HPLC TSQ Quantum Access triple quadrupoleC18 (400 μl min−1)363.1 → 183.2Negative ESI100 μl
4513-0042Method 1 and 2Agilent 1200 binary HPLC TSQ Quantum Access triple quadrupoleC18 (400 μl min−1)353.0 → 285.0Positive ESI100 μl (Quantum)
SordarinMethod 1 and 2BothDiphenyl (200 μl min−1)493.6 → 333.4Positive ESI100 μl (Quantum) 10 μl (Vantage)
TSAMethod 2Refrigerated CTC Pal autosampler, Thermo MS Surveyor pumps TSQ Vantage triple quadrupolePFP (300 μl min−1)303.0 → 148.1Positive ESI10 μl
A77636Method 2Refrigerated CTC Pal autosampler, Thermo MS Surveyor pumps TSQ Vantage triple quadrupolePFP (300 μl min−1)330.2 → 135.2Positive ESI10 μl