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Analytical Facility

The Analytical Facility for the University of Tennessee Health Science Center College of Pharmacy houses 2 NMR spectrometers (500 and 400 MHz) and 4 mass spectrometers as well as a couple of HPLC, UV, IR, and polarimeter instruments. It is the largest available state-of-art analytical and bioanalytical facility for researchers in UTHSC. The facility provides critical analytical/bioanalytical support to a broad spectrum of research in drug discovery including medicinal chemistry, drug metabolism and pharmacokinetics (DMPK), drug delivery, formulation, and other bioanalytical work. 

 

NMR

Instrument
Name
Location Year
Acquired
Probes Image
Varian Inova 500 Pharmacy Bldg Room B024 2001
  • 5mm TRPFG
  • 5mm S/W PFG
  • 5mm Penta PFG
  • 3mm IFC
  • 4mm Nano probe
Varian Inova 500
Bruker Avance III 400 Pharmacy Bldg Room B024 2011 5mm BBO Brunker Avance III

LCMS

Instrument
Name
Location Year
Acquired
Ion source(s)/ Analyzer Image
Waters Xevo G2-S QTOF with waters Acquity UPLC Pharmacy Bldg Room 502  2012 ESI/APCI Quadrupole TOF Waters Xevo
AB Sciex API-4500 with Shimadzu Nexera X2 UPLC  Pharmacy Bldg Room 419 2013 ESI/APCI Triple-Quadrupole AB-Sciex 4500
SCIEX TQ5500 with Shimadzu Nexera XR HPLC Pharmacy Bldg Room 421 2014 ESI/APCI Triple-Quadrupole  SCIEX TQ5500 with Shimadzu Nexera XR HPLC
Bruker amaZon SL Mass Spec with Shimadzu HPLC Pharmacy Bldg Room 502  2016 ESI/Ion Trap Bruker amaZon SL Mass Spec with Shimadzu HPLC
*Waters SYNAPT G2-Si HDMS with ACQUITY M-Class UPLC and Progenesis QIP software  Pharmacy Bldg Room 415 2017 Nanoelectrospray/QTOF with ion mobility *Waters SYNAPT G2-Si HDMS with ACQUITY M-Class UPLC and Progenesis QIP software

Others

Instrument
Name
Location Year
Acquired
Features &
Application
Image
Gilson preparative HPLC Pharmacy Bldg Room 502  2001 UV and Fraction collector Gilson preparative HPLC
Perkin-Elmer FT IR Pharmacy Bldg Room 502  2011 Fourier transform infrared spectroscopy Perkin Elmer
Varian Cary 1E UV Pharmacy Bldg Room B024 1995 UV absorption Varian Cary
Rudolph Aotopol V Polarimeter Pharmacy Bldg Room B024 2013 Optical rotation measurement Rudolph Aotopol

Bruker Avance III 400 MHz

Manufacturer BrukerBiospin (Billerica, MA, USA)
Specifications
  • Nanobay console
  • 400 MHz magnet
  • Bruker SampleCase (autosampler) with 24 sample holders
  • Anti-vibration legs
  • Ultra-shielded and ultra-long hold magnet
  • Variable temperature experiments
  • Automatic Tuning and Matching (ATM)
  • Fully automated operation
Probes
  • 5mm BBO (Broad Band Observe) probe
  • The inner coil is optimized for x-nuclei from15N to 31P and with z-gradient
Software Topspin 3.0 on Windows 7
Applications
  • Routine 1D, 2D NMR
  • Variable temperature experiments (-20 to +80C)
  • Multiple sample acquisition

Waters Xevo G2-S Q-TOF

Manufacturer Waters (Milford, MA, USA)
Ionization modes Positive and negative (ESI and APCI by direct infusion or LCMS, and Solid Analysis Probe)
Analyzer/detector
  • Sensitivity enhancement by Step-wave technology
  • Mass Selective Quadrupole MS
  • Travelling Wave Ion Guide (TWIG) collision cell
  • Orthogonal TOF (Time of Flight)
Operating modes
  • Full scan MS with two point lock mass correction
  • MSe (fragment all ions)
  • MSMS (fragment a selected parent ion)
M/Z range 20-100,000 Da
Resolving power 30,000 FWHM
Mass Accuracy ±1ppm
Inlets Waters Acquity I-Class UPLC including:
  • Sample Manager (holds 2 x 48 vials or 2 x 96-well plates)
  • Binary Solvent Manager (flow range: 0.1 to 2.0/min (gradient))
  • Thermostatted Column Manager
  • PDA (Photo Diode Array) detector
Software Masslynx 4.1 on Windows 7
Applications
  • High-resolution analysis
  • Identification of unknown metabolites
  • Forensics
  • Quantitative analysis of both small and big molecules

AB Sciex API-4500

Manufacturer AB Sciex (Foster City, CA, USA)
Ionization modes Positive and negative (Turbo V source with ESI and APCI) by direct infusion or LCMS
Analyzer Triple quadrupole (QJet® 2 Ion Guide delivers 10x higher sensitivity over API-3000)
Operating modes
  • MS Full-scan (Q1 or Q3)
  • MS/MS Product ion Scan
  • MS/MS Precursor ion Scan
  • MS/MS Neutral Loss Scan
  • Multiple-Reaction Monitoring (MRM)
M/Z range Up to 2000 Da
Resolving power Unit mass resolution
Mass Accuracy ±0.2u
Inlets
  • Shimadzu Nexera X2 UPLC (flow range: from 0.1 to 2.0 mL/min)
  • CTC PAL Autosampler (holds 6 x 48 vials or 96-well plates)

 


Waters SYNAPT G2-Si HDMS with ACQUITY M-Class UPLC and Progenesis QIP software

Manufacturer Waters (Milford, MA, USA)
Ion Source/Analyzer Nanoelectrospray/QTOF with ion mobility
Analyzer QTOF with ion mobility
Performance Attributes
  • Resolution up to 50 000 FWHM
  • Mass accuracy less than 3 ppm
  • Data-independent and data-dependent acquisition
Main Application  Qualitative and quantitative proteomics
Note This instrument is available for collaborative research projects. Please contact Drs. Beranova (sberanova@uthsc.edu) or Giorgianni (fgiorgia@uthsc.edu) to discuss your biological mass spectrometry interests and needs.

Sciex TripleQuad 5500

Manufacturer  Sciex (Framingham, MA, USA)
Ionization Modes Positive and negative (Turbo V source with ESI and APCI) by direct infusion or LCMS
Analyzer  Triple quadrupole (QJet® 2 Ion Guide)
Operating Modes
  • MS Full-scan (Q1 or Q3)
  • MS/MS Product ion Scan
  • MS/MS Precursor ion Scan
  • MS/MS Neutral Loss Scan
  • Multiple-Reaction Monitoring (MRM)
M/Z Range  Up to 1000 Da
Resolving Power Unit mass resolution
Mass Accuracy ±0.2u
Inlets
  • Shimadzu HPLC (flow range: 0.3-0.5mL/min preferred for LC-MS application)
  • Shimadzu SIL20ACXR (1mL or 1.5mL HPLC vials or 96-well plates)

Bruker amaZon SL MS

Manufacturer  Bruker Daltonics (Billerica, MA, USA)
Ionization Modes Positive and negative (ESI) by direct infusion or LCMS
Analyzer  Ion trap
Operating Modes Full scan MS and MSMS
M/Z Range  Up to 2200 Da
Resolving Power Unit mass resolution
Mass Accuracy 0.2 u
Software Compass 1.7 for amaZon with trapControl 7.2, HyStar 3.2, and DataAnalysis 4.2
Applications
  • Low-resolution analysis (nominal mass) for small molecules and peptides
  • Qualitative and quantitative analysis of small molecules
Inlets
  • Shimadzu LC-20AD HPLC 
  • SIL-20A HT autosampler ( up to 105 1.5mL HPLC vials)
  • SPD-20 AV UV/VIS detector
  • CTO-20 AC column oven
  • CBM-20A controller

NMR Policy

  1. Only authorized users can have the key and access to the NMR instrument. Authorized users are defined as trained by Dr. Jianjun Chen, demonstrated capability to work on an instrument and obtained a key from campus police.
  2. NO food and drinks in the NMR lab.
  3. NO gloves on the keyboards.
  4. NO sample preparation in the NMR room.
  5. NO loose metal objects in the NMR room.
  6. Users must sign in the timetable to reserve his/her time during his usage, and write in the logbook after each use. Using the instrument without signing timetable and writing log may result forfeiting his/her access to the NMR room.
  7. If one signs up for a time and later find that one does not need it, one must clear his/her sign up.
  8. While the department will pay for normal repair and maintenance, your supervisor will be responsible for any charge of repair due to your fault. Remember, in NMR, it is very expensive even with the smallest repair.
  9. If you work on the 500 NMR with a non-regular probe (nano probe or flow probe). You must block all the time until the regular solution probe is exchanged. You must also put a sign on the keyboard warning users of the special probe. Failure to do so may result severe damage to the probe and magnet by other users, and this will immediately disqualify you working on the special probe.
  10. If you notice any abnormal symptoms of the instruments, do not use it and inform Dr. Jianjun Chen/Dr. Wei Li immediately.

LCMS Policy

  1. You must be trained by Dr. Jianjun Chen in order to use the LC/MS. No one is allowed to use other people’'s account unless authorized by Dr. Jianjun Chen.
  2. You must reserve your time of usage and record your usage in the log book. If you just use one function (i.e. HPLC or MS), write HPLC only or MS only, so that others can use the other function. When recording your usage, write down the background ions, the solvent you use, and the ions of your compound and problems (if any) of the instrument.
  3. Before you use it, check the logbook to see if the instrument is ok. If you find anything abnormal, DO NOT USE the instrument and report to Dr. Jianjun Chen immediately.
  4. NO food and drinks in the LCMS lab.
  5. NO gloves on the keyboards.
  6. If one signs up for time and later finds that one does not need it, one must clear his/her sign up.
 
Instrument COP users and NIH major users External users (Other departments in UTHSC) Industry users
Waters Xevo G2-S QTOF with waters Acquity UPLC   $10/hour   $30/hour   $80 per sample
Sciex TripleQuad 5500 with Shimadzu HPLC   $25/hour   $75/hour   $90 per sample
AB Sciex API-4500 With Shimadzu Nexera X2 UPLC   $20/hour   $60/hour   $80 per sample
Bruker amaZon SL Mass Spec with Shimadzu HPLC   No charge   $20/hour   $25 per sample
Varian Inova 500   $10/hour *   $30/hour   $50 per sample
Bruker Avance III 400   $10/hour *   $30/hour   $50 per sample
Gilson preparative HPLC   No charge   $30/hour   $50 per sample
Perkin-Elmer FT IR   No charge   $30/hour   $50 per sample
Varian Cary 1E UV   No charge    $30/hour   $50 per sample
Rudolph Aotopol V Polarimeter   No charge    $30/hour   $50 per sample
Scintillation Counter  $10/hour    $30/hour  $60/hour

*For Varian Inova 500 and Bruker Avance III 400: ($6/hr during 5PM-8AM and weekends)

COP users are defined as users for which usage charges are charged to a COP account.

NIH major users are NIH S10 application major users outside COP

Purpose of the policy: This policy is aimed at ensuring the operation and functionally of the shared instrumentation resources within the University of Tennessee College of Pharmacy.  It limits access to specific levels of trained users and establishes user fees for long-term financial stability in the basic operation and maintenance of the equipment.

User access:

Access to the 400 MHz NMR, 500 MHz NMR, and Bruker amaZon Mass Spec is provided to general users with COP or UTHSC affiliation after appropriate training has been received and a user account has been established.

Access to the Xevo G2-S QTOF LCMS and AB 4500 Triple Quad LCMS is provided only to expert users with multiple years or proven experience in mass spectrometry and prior approval.

Specifics for each instrument are regulated by instrument specific policies. 

Mass spectrometry specialist assisted operation:

For the Xevo G2-S QTOF LCMS and AB 4500 Triple Quad LCMS, mass spectrometry specialist assisted operation can be requested at a fee of $ 35/hour for COP users and $ 90/hour for other UTHSC users. Availability is schedule-dependent.

Fee Charges:

Monthly charges are tracked by the COP shared instrumentation manager and are provided to the business manager of the Department of Pharmaceutical Sciences. COP and other UTHSC users have to provide an account to the COP shared instrumentation manager prior to initiation of any work.

For users without current funding, the user fees need to be covered by the responsible department and usage requires prior approval by the department chair.

Prioritization:

Preference for instrument usage is given to COP and NIH major users, followed by other UTHSC users and outside users.

Last Published: Nov 7, 2017