Research & Faculty

Mass Spectrometry / Microanalysis

About

The UBC Mass Spectrometry Centre is a regional facility, providing analytical support for researchers at UBC, at other Universities in the Province, and for various companies. The Centre is equipped with modern analytical instrumentation, providing most of the mass spectrometric techniques currently available.

Contact Information

Yun Ling, Ph. D.
Department of Chemistry
University of British Columbia
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada
Tel: (604) 822-3235 (office)
       (604) 827-4212 (lab)
Fax: (604) 822-2847
Email:

Location

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Laboratory: E313/E315
Lab Phone No. 604-8274212
Department of Chemistry
University of British Columbia
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada

Staff

 

 

 

 

 

 

 

 

 

 

Yun Ling, PhD, Facility Manager
Marshall Lapawa, Research Technician
Derek Smith, Research Technician
Marco Yeung, Research Technician

Instruments

Kratos MS-50

This is a high resolution double focusing sector instrument dedicated for EI. It is used for both low and high resolution mass spec analysis. Accurate mass measurement for EI samples are normally performed on this instrument. The instrument is mainly used for analyzing small non-polar organic compounds and organometallics. Air-sensitive compounds can be analyzed on this instrument.

Kratos Concept IIHQ

This is a high resolution double focusing hybrid mass spectrometer with EBQQ configuration.  Ion source available on this instrument include EI, DCI and LSIMS. The instrument is mainly used for EI, DCI and LSIMS samples. Accurate mass measurements for DCI or LSIMS samples are normally analyzed on this instrument.

Waters/Micromass LCT

This is a time-of-flight (TOF) mass spectrometer equipped with both electrospray (ESI) and atmospheric pressure chemical ionization (APCI) ion source. It has a capability for accurate mass measurements of ESI and APCI ions.  The samples are introduced by infusion.

Bruker HCT

This is an ion trap mass spectrometer equipped with electrospray (ESI) ion source. The sample could be introduced by infusion, flow-injection or on-line HPLC.  MS/MS for ESI samples can be measured on this instrument. Both CID and ETD are available. Agilent HPLC is coupled for LC-MS analysis. The instrument is available for self-operation after training.

Bruker Autoflex MALDI-TOF

This is a time-of-flight mass (TOF) spectrometer equipped with MALDI ion source. It can be operated in either linear or reflectron mode. It is mainly used for routine molecular mass determination for metalloporphrins, supramolecular coordination assemblies, synthetic polymers, and biomolecules. The system is readily learned and operated by students.

Waters LC-MS

The mass spectrometer is Waters ZQ equipped with ESCI ion source. Waters 2695 HPLC is used to deliver the samples. It is mainly used for routine molecular mass determination for polar organic compounds. The system is readily learned and operated by students.

Agilent GC-MS

The mass spectrometer is an Agilent 5977A MSD coupled to 7890B GC. Both EI and CI ion sources are available with the MSD. The GC include a split/splitless inlet and multimode inlet (MMI). MMI is connected to a Thermal Separation Probe (TSP) for direct sample introduction.  It is mainly used for routine molecular mass determination for non-polar organic compounds. The system is readily learned and operated by students.

Thermo Flash 2000 Elemental Analyzer

This is an instrument designed for the determination of total carbon, hydrogen, nitrogen, sulphur and oxygen (C, H, N, S, O) present in a wide range of organic and inorganic samples. Currently CHN and CHNS analysis are available.

Services

Services available
Sample submission and forms
Sample preparation
Training
Booking

Services Available

Mass Spectrometry Services

Ionization Methods

Instruments

Compounds

EI
(Electron Impact Ionization)

Kratos MS-50
Kratos Concept IIHQ
Agilent GC-MS

Non-polar or Less polar Organic,
Organometallics

CI
(Chemical Ionization)

Kratos Concept IIHQ
Agilent GC-MS

Less polar, Polar Organic

LSIMS
(Liquid Secondary Ion Mass Spectrometry)

Kratos Concept IIHQ

Polar Organic
Organometallics

ESI
(Electrospray Ionization)

APCI
(Atmospheric Pressure Chemical Ionization)

Waters/Micromass LCT
Bruker HCT
Waters LC-MS

Polar Organic,
Organometallics
Porphyrins,
Coordination Compounds Peptides and Proteins Oligonucleotides

MALDI
(Matrix-Assisted Laser Desorption/Ionization)

Bruker Autoflex

Porphrins, Metalloporphrins
Metal Coordination Complexes
Supramolecular Coordination Assemblies,
Peptides and Proteins, Carbohydrates, Oligonucleotides,
Synthetic Polymers

LC-MS
(Liquid Chromatography-Mass Spectrometry)

Agilent HP1100
Bruker HCT
Waters LC-MS

Same as ESI / APCI

GC-MS (Gas Chromotography-Mass Spectrometry) Agilent GC-MS Non-polar and less polar organic compounds

 

All mass spectrometric techniques can provide spectra in unit mass format. A molecular mass measurement can be used to determine the molecular weight of a compound, confirming the presence or absence of a compound. High resolution accurate mass measurements are available for some ionization modes (EI, ESI, and APCI). Accurate mass measurement of small molecules is used to verify a predicted molecular formula of a pure compound. MS/MS measurements are available for ESI and APCI. MS/MS spectra could be used to provide structure or sequence information of a compound.

Elemental Analysis Service

CHN and CHNS determinations are available. The analysis is mainly used to verify a formula or purity of a compound. See details for sample submission of Elemental Analysis.

Sample Submission and Forms

Please submit the samples to E313 in the chemistry north wing. There is different sample form for different analysis at E313. Users are asked to fill the sample submission form and log form. The required information for each technique on the submission form should be filled as much as you could, especially proposed molecular formula, molecular weight, sample stability and required special handling. The same MS/MA # and sample name for each sample should be in the log form, sample submission form and on your sample vial.  Sample vials should be put in the correct sample holder. A refrigerator is available for storing samples at 2 and -6°C. For most compounds, milligram amounts are preferred although micrograms are sufficient.

Please contact lab manager before submission or shipment of sensitive or potentially hazardous materials requiring special handling on arrival.

No toxic and radioactive sample is accepted.

 

Electron Impact Ionization (EI)

Samples submitted for EI analysis (EI Low Res Form) will be analyzed on Kratos MS-50. The sample should be submitted as solid or neat liquid. Air-sensitive sample should be specified on the sample form. Air-sensitive sample analysis is currently only available on MS-50. A minimum of 0.01 mg sample is required. Sample can be analyzed on Agilent GCMS as well.

Samples submitted for high resolution EI analysis (EI High Res Form) will be first analyzed by low resolution EI to determine if the mass to be measured for the expected compound is found. More samples are required for high resolution mass measurements. Or users are asked to provide a low resolution EI MS.

 

Chemical Ionization (CI)-N/A currently

Samples submitted for CI analysis will be analyzed on Agilent GCMS. Sample should be submitted as solid or neat liquid.

The commonly used reagent gases for CI include ammonia, methane and isobutane. The current reagent gas is methane.

Liquid Secondary Ion Mass Spectrometry (LSIMS)-N/A currently

Samples submitted for LSIMS analysis will be analyzed on Kratos Concept IIHQ instrument. The sample should be submitted as solid or neat liquid.

Samples submitted for high resolution LSIMS analysis will be analyzed by low resolution LSIMS to determine if the mass to be measured for the expected compound is found and to confirm the choice of the matrix. The commonly used matrices include glycerol, thioglycerol and 3-nitrobenzylalcohol.

Electrospray Ionization (ESI)

Samples submitted for low resolution ESI (ESI Low Res Form) will be usually analysed on Bruker HCT instrument. The sample could be solid or liquid. Solid samples are preferred. If submitted in solution, it should be dissolved in 0.5 ml of a solvent that is appropriate for the sample at a concentration 10-100 µM. We would prefer concentrated solution so we could dilute it to working concentration. The solvent must be specified, or solubility information must be provided. The solvents should be electrospray compatible. Some of common used solvents include methanol and acetonitrile. Solvents that should be avoided include DMSO, DMF and THF. Methanol would be the default solvent if no solvent information is specified. All salts should be avoided. Salts and buffers are in general detrimental to MS analysis and may cause ionization suppression especially for ESI-MS. Be sure to indicate if the compound is sensitive to acid or basic condition.

Samples submitted for high resolution ESI analysis (ESI High Res Form) will be analyzed on the Waters/Micromass LCT TOF-MS. The sample will first be analyzed by low resolution ESI to determine if the mass to be measured for the expected compound is found and to confirm the choice of the solvent.

Samples submitted for ESI MS/MS analysis (MS/MS Form) will be analyzed on the Bruker HCT instrument. The sample will first be analyzed by low resolution ESI to determine if the mass of the expected compound for MS/MS analysis is found and to confirm the choice of the solvent.

 

Matrix-Assisted Laser Desorption/Ionization (MALDI)

Samples submitted for MALDI analysis (MALDI-TOF Form) will be analysed on Bruker autoflex MALDI-TOF instrument. The sample should be dry solid. If submitted in solution, protein and peptide samples should be prepared at a concentration of 20-100 µM in water or acetonitrile. Oligonucleotide sample should be prepared at higher concentration (100- 400 µM). A 20 µl sample solution should be sufficient for analysis in most cases. Synthetic polymer should be prepared at even higher concentration, 200-1000 µM. Salts and buffers are in general detrimental to MS analysis. Salts or buffer may interfere with the matrix crystallization resulting in signal suppression. Salts may also form adduct that cause peak broadening in reduced mass accuracy and signal intensity. It is recommended that the concentration of salts and buffer should be less than 10 mM. The use of non-volatile agents such as salts and should be avoided.

Solvent–free MALDI is available for insoluble synthetic polymers or supramolecular complexes.

 

Gas Chromatography-Mass Spectrometry

Sample submitted for GC-MS analysis (GC-MS From) will be analyzed on Agilent GC MSD. Using 2mL autosampler sample vial. Solvent should be high purity volatile organic solvents - non-polar solvents preferred. Typical concentration is 1 to 100ppm. Solid sample can be run using the Thermal Separation Probe (TSP).

 

Liquid Chromatography-Mass Spectrometry

Samples submitted for LC-MS analysis (LC-MS Form) will be analyzed on Agilent HP1100 / Bruker Esquire~LC instrument. User would be required to provide HPLC column as well as HPLC conditions such as solvent, suggested gradient, flow rate and a HPLC chromatogram under the suggested condition. Contact lab manager for details.

Elemental Analysis

Samples submitted for CHN and CHNS analysis (EA Sample Form) will be analysed on Thermo Flash 2000 elemental analyzer. Elemental analysis should be one of the last analytical techniques for compound characterization. Sample of high purity (98-99%) should be submitted; otherwise the measured values would not be useful. The identity of the sample should be confirmed by other techniques such as mass spec before submitting to EA.  The minimum amount of solid or liquid sample should be 5 mg for CHN and 10 mg for CHNS analysis Air-sensitive and hydroscopic sample should be submitted in Schlenk tube and specified on the sample form. Air-sensitive samples should be scheduled ahead of time with the EA analyst or lab manager.

Samples such as soils, rocks, inorganic materials, etc, are unacceptable since their decomposition will leave large amounts of residue that may interfere with subsequent determinations.

For more information, please refer to this Summary

Air-sensitive samples

It is important that you set up a time for analysis with staff personnel ahead of time. Air-sensitive samples for EI analysis are currently analyzed on Kratos MS-50 instrument.

Air-sensitive samples requiring ESI and/or MALDI need to be organized with one of staff members. Please contact mass spec lab personnel for detailed procedure.

 

High resolution mass spec service

Samples submitted for high resolution mass spec analysis should be relative pure. So-called high res mass spec analysis for small molecules is actually accurate mass measurement on the mass of interest normally performed on high resolution mass spectrometer. The mass of interest is measured with enough accuracy to limit the possible elemental compositions or confirm unique composition. The mass to be measured must be confirmed in low res full scan before submitted for high res MS. The sample does not have to be pure, but the mass of interest needs to be intense enough for the measurement and must be separated from interference of other masses. Students are encouraged to look at their low resolution full scan spectra before proceeding with the request for high res MS. The compound of interest should be purified; this will avoid and /or minimize possible ionization suppression and ensure the ion intensity of the analyte, especially for ESI-MS. The mass to be measured should be confirmed as base peak or comparable to the base peak in the low res spectra, especially for those obtained from open access ESI/APCI MS.  An exception is given to a compound for which the molecular ion is not detected as base peak because of fragile structure.

 

Sample preparations for Self-Serve MS.

  • Sample preparation for open access API (ESI/APCI)-MS.
    • Must use only standard 2mL autosampler sample vials with proper septa (from Waters or equivalent). (Available from Chem Stores). Wrong sample vial could damage the sample management system.
    • Default solvents include methanol, acetonitrile and water.
    • Any solvent used to dissolve the sample must be miscible to one of three recommended solvents. Avoid use involatile solvents and buffers such as DMSO, DMF, phosphates, DCM. If these solvents are required to dissolve the sample, make every effort to use some, even up to 50%, one of three recommended solvent in each sample vial.
    • Recommended solution concentration range: 10µM to 100µM.
    • Recommended volume of sample solution should be 1.0-1.5mL. Low volume inserts are needed for low volume sample solution.
    • Must filter sample solutions if they are cloudy or display visible precipitates.
    • Please label your sample vial with sample id.
  • Sample preparation for Self-Serve ESI/APCI-MS on Bruker HCT. (Similar as for OA-MS).
  • Sample preparation for Self-Serve MALDI-MS.

Samples for MALDI-TOF analysis need to meet certain requirements for obtaining good spectra. The more careful you prepare samples, the more likely a successful analysis will be. Here are some guidelines.

  • Avoid using non-volatile reagents salts, detergents and solvents.
  • Purify samples.
  • Use volatile solvents include methanol, acetonitrile and water.
  • The total amount of sample needed for MALDI analysis depends on the sample type.
  • Stock solution for supramolecular complexes should be 1mg/mL and 10 mg/mL for synthetic polymers. Working solution can be made by the dilution of stock solution with matrix solution (saturated) at different ratios.
  • Same solvent should be used for sample, matrix and cationizaion reagent.
  • Cationization reagent should be used for synthetic polymers.
  • Two standards should be used for mass calibration and should cover range of analyte masses.

Training for Self-Serve MS.

User may be trained to run four self-serve instruments. Training can be scheduled as needed.

FAQ

Mass Spectrometry Services

  • How do I submit an air-sensitive sample for mass spec analysis?
    • Air-sensitive samples for EI analysis will be analyzed on Kratos MS-50 instrument.
      Air-sensitive samples requiring ESI and/or MALDI need to be organized with one of staff members. Arrangements can be made to analyze your sample immediately upon arrival at an agreed-upon time. We may ask you to prepare the sample solution in your glovebox and bring it to the mass spec lab in special "packaging" along with a small amount of rigorously dry, degassed solvent.

Elemental Analysis Service

  • How much sample do I need to submit?
    • About 5 mg sample should be submitted for CHN analysis and 10 mg for CHNS analysis. Normally 1-2mg will give a good result for CHN analysis (3-4 mg for S analysis). But extra sample is required for possible rerun.
  • How do I submit air-sensitive samples for EA analysis?
    • It is important that you set up a time for analysis with staff personnel ahead of time. Please contact lab manager or EA analyst for detailed procedure.

Self-Serve MS Services

  • What could be the reasons for the target mass not confirmed on the printout?
    • Data processing error
    • Wrong method used
    • Ion suppression
  • How do I get training?
    • Users may be trained by facility staff to run OAMS, GC-MS, ESI-MS and MALDI.
      Training is scheduled as needed. Contact Yun Ling at

High Resolution Mass Spectrometry

  • What is high resolution mass spectrometry service?
    • So-called high resolution mass spectrometry service is the accurate mass measurement on the masses of interest. Accurate mass measurements are used to determine the elemental composition for molecular or fragment ions. These measurements are performed normally on high resolution mass spectrometer so that the masses are measured for a single species and not measured for unresolved or partially resolved peaks. The masses of interest are measured with enough accuracy to limit the possible elemental composition or confirm unique composition. The term “high resolution” is often used interchangeably with “accurate mass”, but the terms really refer to two different things.
  • Requirements for high resolution mass spec samples
    • Only submit the samples if
      • The compound has been purified; this will avoid /minimize possible ionization suppression and ensure the ion intensity of the analyte.  Peak of interest for the ion detected on OAMS should have minimum signal/noise (S/N) ratio of 10.
      • The mass for the ions formed from the compound is confirmed – use exact mass, not molecular weight.
      • Correct isotope pattern for the compound is detected.
      • The possible elemental composition for the compound is proposed.
  • Why would the samples be returned?
    • The samples will be returned if it is impossible to measure the mass of interest or the measured mass is not meaningful.
      • The mass assigned for the peak to be measured is wrong for the formula proposed, or no mass has been specified to be measured.
      • The intensity of the peak chosen for the measurement is too weak to be measured.
      • Sample provided is not enough. Minimum sample required is 300 µl solution of 100uM.
      • Wrong isotope pattern is detected. This would suggest that a different compound is detected or there are overlaps due to the different compounds.
      • No elemental composition information is provided.
      • Low res spectrum has not been included with the sample form.

ASMS Conference Abstract

ASMS2003 (PDF)

ASMS2004 (PDF)

ASMS2005 (PDF)

ASMS2006 (PDF)

ASMS2007 (PDF)