Chemically synthesized Heparin-like oligosaccharides

Responsible:

Rebecca Miller . University of Oxford . becky@liv.ac.uk

Sample preparation

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1.Sample Origin

General information:
Chemically synthesized Heparin-like oligosaccharides

Growth/harvest conditions for recombinantly produced material:
N/A

Treatments and/or storage conditions:
NA

For commercial material, vendor and applicable item information:
N/A

Generation of chemically derived material:
DOI: 10.1002/chem.201204519 Synthesis of a Targeted Library of Heparan Sulfate Hexa- to Dodecasaccharides as Inhibitors of b-Secretase: Potential Therapeutics for Alzheimer's Disease. DOI: 10.1002/chem.201204519

2. Sample Processing

Purification steps:
NA

2. Defined Sample

Sample name:
Glycosaminoglycans

HPLC

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N/A

MS

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1. General features

Date stamp: Thu Jul 26 UTC 2018

Instrument: Waters Synapt MS QTOF

Customizations from the manufacturer's specification:
NA

ion_mode: -

2. Ion sources

(a) Electrospray ionisation - ESI

Sprayer type : Static

Interface name: NA

Other data for the Interface: NA

Sprayer name: Gold plated tips

Other data for the sprayer: Borosilicate electrospray tips made in house. Briefly, the borosilicate tubes (no. 1B120F-4) were purchased from World Precision Instruments, Inc. (Sarasota, FL), and were pulled using a Sutter P97 Flaming/Brown micropipette puller (Ringmer, Sussex, UK). The tips were gold coated using a Quorum Technologies SC7640 sputter coater (Ringmer, Sussex, UK).

Relevant voltages: Capillary Voltage - 0.55 kV, sample cone - 7V, cone voltage - 0.6 V Source Temp – 40 oC, Trap CE – 1.0 V, Transfer CE - 3.7 V, Source (ml / min) – 0, Trap (ml / min) – 1.0, IMS (ml / min) – 20.8, LM Resolution – 4.7, Trap DC Entrance – 1.0 V, Trap DC Bias – 10 V, Trap DC Exit – 5.0 V, IMS DC Entrance – 1.5 V, IMS DC Exit – 2.0 V, Transfer DC – 5.0 V, Transfer DC Exit – 1.0 V, Source Wave Velocity – 300 m/s , Source Wave Height – 0.2 V, Trap Wave Velocity – 300 m/s, Trap Wave Height – 0.2 V, IMS Wave Velocity – 370 m/s, IMS Wave Height – 8.0 V, Transfer Wave Velocity – 320 m/s, Transfer Wave Height – 4.2 V, Mobility Trapping Release Time – 100 µs, Mobility Trapping Trap Height – 10 V, Mobility Trapping Extract Height – 5 V.

Degree of prompt fragmentation evaluated: Yes

In-source dissociation performed: No

Other parameters if discriminant for the experiment: NA

(b) MALDI

Plate composition (or type): NA

Matrix composition: NA

Deposition technique: NA

Relevant voltages: NA

Degree of prompt fragmentation evaluated: NA

PSD (or LID/ISD) summary: NA

Operation with or without delayed extraction: NA

Laser type: NA

Other laser related parameters: NA

url: NA

3. Ion transfer optics

Hardware options: NA

3. Post-source componentry

Collision-Induced Dissociation - CID

CID. Gas composition: NA

CID. Gas pressure: NA

CID. Collision energy: NA

Electron Transfer Dissociation - ETD

ETD. Reagent gas: NA

ETD. Pressure: NA

ETD. Reaction time: NA

ETD. Reagent atoms: NA

Electron Capture Dissociation - ECD

ECD. Emitter type: NA

ECD. Voltage: NA

ECD. Current: NA

TOF drift tube

TOF. Reflectron status: NA

Ion Trap

Ion trap. Final MS stage achieved: NA

Ion mobility

Ion mobility. Gas type : Helium

Ion mobility. Pressure: NA

Ion mobility. Instrument parameters: Shown above

FT-ICR

Peak selection: NA

FT-ICR. Pulse: NA

FT-ICR. Width: NA

FT-ICR. IR: Decay time: NA

FT-ICR. IR: NA

FT-ICR. Other parameters: NA

Detectors

Detector type: NA