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MB Sample ID: SA088395

Local Sample ID:CA209038-8-48_week 6
Subject ID:SU001303
Subject Type:Human
Subject Species:Homo sapiens
Taxonomy ID:9606

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Subject:

Subject ID:SU001303
Subject Type:Human
Subject Species:Homo sapiens
Taxonomy ID:9606

Factors:

Local Sample IDMB Sample IDFactor Level IDLevel ValueFactor Name
CA209038-8-48_week 6SA088395FL012979week 6Time point
CA209038-8-48_week 6SA088395FL0129791OS_Censor (1 means the time is a censoring time and 0 means a failure time in OS)

Collection:

Collection ID:CO001297
Collection Summary:Serum was collected at the specified time-points by centrifugation at 4000g for 4 minutes at 25°C within 2 hours of collection. Samples were frozen immediately and stored at or below -20°C for up to two months followed by storage at -80°C.
Sample Type:Blood (serum)
Storage Conditions:Described in summary

Treatment:

Treatment ID:TR001318
Treatment Summary:Serum samples were obtained from 78 participants in the the nivolumab monotherapy arm of CA209-038 (NCT01621490), a multi-institutional, multiarm prospective trial investigating the pharmacodynamics of nivolumab in patients with unresectable or metastatic melanoma.
Treatment Protocol ID:NCT01621490

Sample Preparation:

Sampleprep ID:SP001311
Sampleprep Summary:Serum samples (10 µL) were extracted using 90 µL of 74.9:24.9:0.2 (v/v/v) acetonitrile/methanol/formic acid containing stable isotope-labeled internal standards (0.2 ng/µL valine-d8, Isotec; 0.2 ng/µL phenylalanine-d8, Cambridge Isotope Laboratories). The samples were centrifuged (10 min, 9000g, 4ºC) and the supernatants were transferred to autosampler vials with de-activated inserts (Waters). Factors: OS_Censor (1 means the time is a censoring time and 0 means a failure time in Overall Survival)

Combined analysis:

Analysis ID AN002053
Analysis type MS
Chromatography type HILIC
Chromatography system Agilent 1290 Infinity II
Column Waters Atlantis HILIC (150 x 2.1mm)
MS Type ESI
MS instrument type Triple quadrupole
MS instrument name Agilent 6495 QQQ
Ion Mode POSITIVE
Units Log10(Peak Area)

Chromatography:

Chromatography ID:CH001492
Chromatography Summary:Extracts (10 µL) were injected onto a 150 x 2.1 mm Atlantis HILIC column (Waters). The column was eluted isocratically at a flow rate of 250 µL/min with 5% mobile phase A (10 mM ammonium formate and 0.1% formic acid in water) for 1 minute followed by a linear gradient to 40% mobile phase B (acetonitrile with 0.1% formic acid) over 10 minutes
Instrument Name:Agilent 1290 Infinity II
Column Name:Waters Atlantis HILIC (150 x 2.1mm)
Column Temperature:30
Flow Rate:250 µL/min
Solvent A:100% water; 0.1% formic acid; 10 mM ammonium formate
Solvent B:100% acetonitrile; 0.1% formic acid
Chromatography Type:HILIC

MS:

MS ID:MS001905
Analysis ID:AN002053
Instrument Name:Agilent 6495 QQQ
Instrument Type:Triple quadrupole
MS Type:ESI
MS Comments:MS data were acquired using multiple reaction monitoring. Retention times, mass transitions, and collision energies were determined using authentic reference standards. Other MS parameters were: ion spray voltage, 3.0 kV; source temperature, 200°C; nozzle voltage, 500 V; gas flow, 14 L/min; nebulizer, 40 psi; sheath gas, 250°C; sheath gas flow, 1 L/min; iFunnel high pressure RF, 90; and low pressure RF, 90. Raw data were processed using MassHunter software (Agilent, Santa Clara, CA) for automated peak integration. The peak areas of 106 targeted metabolites were manually reviewed for quality of integration and compared against standard reference standards to confirm identities.
Ion Mode:POSITIVE
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