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Chemical Purification Analysis and Screening core facility (CPAS)

OVERVIEW

CPAS operates in self-service mode and offers training for instrument usage in analytical chemistry, mainly for chromatographic separation and purification (LC, GC). Various detection tools are available such as mass spectrometry (MS), flame ionization detection (FID), electron capture detector (µECD), evaporative light scattering detection (ELSD), UltraViolet (UV, UV-Vis) for detection, identification and quantification (MPLC-UV, HPLC-UV/ESLD, UHPLC-DAD, LC-MS-DAD SQ, LC-MS QqQ, LC-MS QTOF, LC-MS triple TOF, GC-FIDs, GC-MSD-µECD, TDU-GC-MSD [HS-SPME], and GC-MS QTOF [HS-SPME]). CPAS also has available ion-mobility spectrometry (IMS) coupled with liquid chromatography (LC), diode array detector (DAD) and high-resolution Mass spectrometry (HRMS) and accurate MS/MS) for a powerful multidimensional separation, detection and identification (LC-DAD-IM QTOF) of complex mixtures. Our core facility also includes Matrix-assisted laser desorption/ionization (MALDI TOF/TOF) mass spectrometry (HRMS, MS/MS and imaging), circular dichroism (CD, VCD), Optical Rotatory Dispersion (ORD), general spectroscopic characterization (UV, FTIR), lyophilization (benchtop and general purpose freeze-dryer), extraction (microwave reactor), synthesis (microwave reactor, hydrogenation apparatus), as well as binding affinity measurement (Microscale Thermophoresis [MST]). CPAS instruments are available 24/7 in self-service mode upon reservation for trained users.

• Contact & Billing
• Usage Fees
• Information Poster
• Mass Spectrometry Analysis Form
• Acknowledgement Co-Authorship

USF CPAS EQUIPMENT AND SERVICES (NES 406 and IDRB 318)

CPAS, NES 406

Agilent GC-MSD 5977B

• Ionization: - Electron impact (EI); Chemical ionization (NCI/ PCI)
• Mass range: - 1.6 – 1050 m/z
• NIST library 2017
• Inlet system: - Agilent 7890B GC
• Analytes: - low molecular weight range, semi-volatile, low-bowling point, non-polar molecules
• Gerstel MultiPurpose Sampler (MPS):
  • Dual headed for sample preparation
  • 10uL syringe, HS/ 2.5mL syringe and HS SPME fiber
  • Cooled Injection System (CIS) allowing cryo-focusing (LN2)
  • Thermal Desorption (TDU) and Thermal Extraction using Automated Liner Exchance (ALEX) for:
    • Twister/ Stir Bar Sorptive Extraction SBSE
    • Thin Film (TF-SPME)
    • Desorption liner (absorbent for air sampling)

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Agilent GC-FID 

• Flame Ionization Detector (FID)
• 16-sample turret for liquid injection
• Split/splitless inlet system: - Agilent 7890B GC
• Low polarity, low boiling point small molecules
• GC#1 standard column
• GC#2 chiral column

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Dionex ultimate 3000 UHPLC DAD

• Detection: - Ultimate 3000 Diode array detector (DAD)
• UV range: - 190- 800 nm
• Inlet system: - Thermo Scientific Dionex Ultimate 3000 UHPLC+ focused with automated fraction collector (AFC)
• Analytes: - wide range of chemical analytes, from small molecules to biomolecules

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JASCO Model J-1500 Circular Dichroism Optical Rotatory Dispersion (CD/ ORD)  spectrometer

• Electronic CD (ECD)/ORD using UV-Vis spectroscopy 
• Simultaneous Multi-Probe: CD, LD, HT, DC, absorbance 
• Walength range 163 to 950 nm
• Light Source: Xenon lamp
• Cuvette: 10 and 1 mm pathlength
• Peltier thermostatted 6-position automatic cell changer
• Microsampling (2 mL, 10 mL samples)
• Capillaries (5 mL samples) for cell in thermostatted Peltier
• Diffuse-reflectance CD (DRCD) for solid state sample measurements
• Determine the absolute configuration of chiral molecules, secondary structure, folding and binding properties of proteins

Biotools ChiralIR-2Xâ„¢ Vibrational Circular Dichroism (VCD) spectrometer

• Simultaneous IR and VCD signal measurements
• Internal Dual PEM (Photoelastic Modulators) 
• Biocell (solution)
• SyncRoCell (rotating cell ideal for solid state measurements)
• TempCon-2X (Peltier temperature controller for cell)
• Determine the chiral properties of small organic molecules, peptide, proteins 

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CPAS, IDRB 318

• Agilent 7890A GC-MS QToF 7200
• Agilent 1260 Preparative HPLC-DAD-MS SQ 6120
• Teledyne-Isco MPLC (UV) and Shimadzu HPLC (UV, ELSD, RID)
• Pion Inc. Parallel Artificial Membrane Permeability Assay (GIT, BBB, Skin PAMPA)[N/A]
• Pion Inc. Solubility evaluation [N/A]

• TECAN Infinite M 1000 Pro microtiter plate reader and Freedom EVO 150 liquid handler [N/A]

• Anton Paar Monowave Reactor 300
• Agilent Cary 60 UV-Vis Spectrophotometer and FTIR 630 Spectrometer
• Labconco Freezone, SP Scientific General Purpose Freeze Dryer (GPFD), rotary evaporators and other concentrators 
• Innovatice Technologies Pure Solv Micro solvent purification system for anhydrous solvent preparation

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Agilent LC-IM QTOF 6560

• Primary ionization: - Agilent Jet-stream Electrospray Ionization (AJS ESI ± ve)
• Complementary ionization: - Atmospheric Pressure Chemical Ionization Source (APCI)
• Mass range: - up to 20,000 amu for the TOF, up to 4,000 for the Quad
• TOF Mass Resolution: FWHM > 22,000 at m/z 1522 independent of acquisition rate
• Inlet system: - Agilent Infinity II 1290 HPLC with infinity III 1260 DAD (190-640nm)
• IM-MS technology: drift tube design that allows direct measurement for accurate collision cross sections (CCS).
• Analytes: - Organic, pharmaceuticals, natural products, peptides, proteins, large biomolecules
• Software: - Open lab Mass Hunter workstation (qual, quant), Bioconfirm, Chemvista, PCDL, Explorer, Profinder, Mass profiler Professional (MPP), lipid annotator, Molecular Structure correlator (MSC), IMS-MS browser, PNNL, high resolution demultiplexing (HRdm 2.0) software, Mass Profiler
• Studies: - HRMS and accurate mass MS/MS analysis of complex mixtures for identification of known and unknown, IMS-MS for the separation of isomers and structural group of compounds, ideal for complex studies such as untargeted screening, metabolomics and lipidomics analyses

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Bruker UltraFleXtreme MALDI- TOF/TOF

• Smartbeam II, 2 GHz for MS and 1 GHz for MS/MS
• FlashDetectorâ„¢ with 5 GS/s 10 bit digitizer for enhanced dynamic range
• Resolution > 45,000
• Analytes: - Protein, peptide, lipids, natural products and polymer
• Software: - FlexControl, FlexAnalysis, FlexImaging
• Supporting Software: Biotools, Polytools, SCiLS Lab

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Nanotemper MicroScale Thermophoresis (MST) Monolith

• Molecular interaction, binding affinity measurements (Kd)
• Fluorescence channels: RED & BLUE
• Dynamic range 1nM to uM
• Up to 24 samples/ run
• Small molecules, proteins, DNA, …

Paar Shaker Hydrogenation Apparatus Model 3921

• Explosion Proof Motor and Switch
• 1L shaker bottle
• Treating chemicals with hydrogen in the presence of a catalyst (60 PSI)
• Catalytic hydrogenation, reduction or condensation for organic synthesis

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