Core Facilities

Chemical Purification Analysis and Screening core facility (CPAS)

Laurent Calcul

Laurent Calcul, Ph.D. (Director)

calcul@usf.edu  (preferred method)
Phone NES 406/IDRB 318: (813) 974-6031
Fax: (813) 974-3203

Need a Reservation? Please Check the Instrument availability below:

OVERVIEW

CPAS operates as a self service core facility and offers its expertise in chromatographic separation and purification (MPLC, HPLC, UHPLC), mass spectrometry detection, identification and quantification (LC-MS SQ, LC-MS QqQ, LC-MS Triple TOF, TDU-GC-MSD, GC-MSD-uECD and GC-MS QTOF [HS-SPME] and MALDI TOF). The services also include 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), ADME screening (Parallel Artificial Membrane Permeability [PAMPA - GIT, BBB and skin] and drug solubility evaluation), binding affinity measurement (Microscale Thermophoresis [MST]), and high-throughput screening development capability (liquid handling robot and multimode plate reader). CPAS provides trainings and instruments are available 24/7 in self-service mode and upon reservation for trained users.

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

CPAS, NES 406

Agilent LC-MS QToF 6540

Shimadzu LC-MS Triple TOF AB Sciex 5600

  • Ionization: ESI (+/-), APCI sources available
  • Resolution: high-resolution with 100 Hz acquisition speed
  • Accuracy: stable ~1 ppm mass accuracy over days of acquisition
  • Scan Speed:  100 Spectra/sec
  • Inlet system:  Shimadzu Nexera 2, LC30AD
  • Analytes:  Organic, Peptides, Proteins, Natural products, metabolomics quantification and identification capabilities
  • Software: Analyst, PeakView, MultiQuant
  • Studies: accurate mass analysis for HRMS/MS

 

Agilent LC-MS QqQ 6460

Agilent LC-MS QqQ 6460

  • Ionization: - Agilent Jet-stream Electrospray Ionization (ESI ± ve) and thermal gradient
  • Sensitivity: - High sensitivity (Femtomole to Attomole range)
  • Inlet system: - Agilent 1260 HPLC
  • Analytes: - Organic, Peptides, Proteins, Natural products, metabolomics and metabolite identification
  • Software: - Mass Hunter workstation
  • Studies: - Tandem mass spectrometry (SRM, MRM) for quantification analysis

 

Agilent LC-MS SQ 6120

Agilent LC-MS SQ 6120

  • Ionization: - Electrospray (ESI ± ve); Atmospheric pressure chemical ionization (APCI ± ve)
  • Mass range: - 10 – 2000 m/z
  • Inlet system: - Agilent 1100 HPLC with Diode Array Detector (DAD)
  • Analytes: - Organic, peptides, Natural products and non-polar compounds

 

Agilent GC-MS SQ 5977B

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)
image 1 image 2 image 3

 

micro

Agilent GC-MSD 5977B/ uECD 

  • Ionization: - Electron impact (EI); Chemical ionization (NCI/ PCI)
  • Mass range: - 1.6 – 1050 m/z
  • NIST library 2017
  • 150-sample tray for liquid injection
  • 2-inlet system: - Agilent 7890B GC
  • Multi-mode inlet (MMI) allowing cryo-focusing (LCO2) connected to MSD
  • Split-splitless inlet (SSI) connected to Electron captor detector (ECD) for manual injection
  • Analytes: - low molecular weight range, semi-volatile, low-bowling point, non-polar molecules, halogenated compounds
d

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

 

cd

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

Biotools ChiralIR-2X™ 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 

CPAS, IDRB 318

paar

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

 

Bruker UltraFleXtreme MALDI- TOF/TOF

Bruker UltraFleXtreme MALDI- TOF/TOF

  • Smartbeam II, 2 GHz for MS and 1 GHz for MS/MS
  • FlashDetector™ 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
nano

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, …
  • JOVE MST link.