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Trinity College DublinSchool of Chemistry16 Dec 2009 Welcome To the Mass Spectrometry Unit Dr. Martin Feeney Room 0.5 Dr. J. Bernard Jean-Denis Chemistry.

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Presentation on theme: "Trinity College DublinSchool of Chemistry16 Dec 2009 Welcome To the Mass Spectrometry Unit Dr. Martin Feeney Room 0.5 Dr. J. Bernard Jean-Denis Chemistry."— Presentation transcript:

1 Trinity College DublinSchool of Chemistry16 Dec 2009 Welcome To the Mass Spectrometry Unit Dr. Martin Feeney Room 0.5 Dr. J. Bernard Jean-Denis Chemistry building

2 Trinity College DublinSchool of Chemistryp 1 1.Introduction to mass spectrometry 2Introduction to mass spectrometry 2. Sample Preparation 7Sample Preparation a. Choice of Solvents b. Sample Solubility c. Sample Concentration d. Sample Vials e. Things to avoid in Sample Prep. 3. Sample submission form 9Sample submission form a. Sample ID b. Proposed Structure c. Sample Handling/Storage 4. Results 12Results 5. MS queries 13MS queries Table of Contents

3 Trinity College DublinSchool of Chemistryp 2 Introduction 1.Introduction to mass spectrometry a- ESI- TOF-MS b- GC- TOF-MS c- LDI-Q-TOF-MS d- ESI-LIT-MS 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries There are a number of instruments in the mass spectrometry facility of the School of chemistry that can offer a wide range of techniques and experiment types, such as MS/MS experiments or mass accuracy determination MS/MS experiments offers structural information of the molecule TOF, Time-of-flight ESI, Electrospray ionisation MALDI, Matrice assisted laser desorption ionisation LIT, Linear ion trap TechniquesInstrumentationsManufacturerMass accuracy MS/MS LC-ESI-TOF- MSLCT ClassicWatersYesNo GC-TOF-MSGCT PremierWatersYesNo MALDI-QTOF-MSMaldi-Qtof PremierWatersYes LC-ESI-LIT-MSAPI 2000Applied Biosystems NoYes

4 Introduction Principle An electric field sufficiently intense to disperse analyte solution emerging from the spray needle into a fine spray required a potential difference of up to sereval kV between that tip and the orifice leading into the vacuum system. The ions will be separate according to their mass-to-charge ratio through a TOF mass analyser before the determination of the accurate mass. 1.Introduction to mass spectrometry a- ESI- TOF-MS b- GC- TOF-MS c- LDI-Q-TOF-MS d- ESI-LIT-MS 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries Trinity College DublinSchool of Chemistryp 3 Sample characteristics Charged or partially charged polar compounds. Sample might need ionisation agent, such as NaCl, Ammonium acetate,... Solvent choice -> see page 7 ESI- TOF-MS ElectroSpray Ionisation coupled to Time-Of-Flight mass spectrometer References: Dole M et al., J. Chem. Phys., 49 (5), p2240. Fenn JB et al., Anal. Chem., 57(3), pp Wiley WC & McLaren IH, Rev. Scientific Instruments, 26, (12), pp LCT Classic, Waters

5 Introduction 1.Introduction to mass spectrometry a- ESI- TOF-MS b- GC- TOF-MS c- LDI-Q-TOF-MS d- ESI-LIT-MS 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries Trinity College DublinSchool of Chemistryp 4 Principle The sample coming from GC effluent could be ionised by three ionisation methods, which are EI (Electron Impact), CI (chemical Ionisation) and FD (Field desorption). The ions will be separate according to their mass-to-charge ratio through a TOF mass analyser before the determination of the accurate mass. Sample characteristics Sample must be thermally volatile and stable Low mass range (typically lower than m/z 650) Solvent choice -> see page 7 GC- TOF-MS Gas Chromatography coupled to Time-Of-Flight mass spectrometer References: Lampman GM et al., Spectroscopy, International Edition, 4 th edition. Wiley WC & McLaren IH, Rev. Scientific Instruments, 26, (12), pp GCT Premier, Waters

6 Introduction 1.Introduction to mass spectrometry a- ESI- TOF-MS b- GC- TOF-MS c- LDI-Q-TOF-MS d- ESI-LIT-MS 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries Trinity College DublinSchool of Chemistryp 5 Principle The sample will be mix with a matrix*. Then, A laser will desorb the mixture and generate ions with high kinetic energy. The ions will be separate according to their mass-to-charge ratio through a TOF mass analyser before the determination of the accurate mass. MS/MS experiments can be done. Possibility of using ESI. * DCTB, CHCA, DIT, DHB. Sample characteristics Generally speaking, samples which could not be ionised by ESI and non volatile Solvent choice -> see page 7 LDI- TOF-MS Laser Desorption Ionisation coupled to Time-Of-Flight mass spectrometer References: Lampman GM et al., Spectroscopy, International Edition, 4 th edition. Wiley WC & McLaren IH, Rev. Scientific Instruments, 26, (12), pp MALDI Q-TOF, Waters

7 Trinity College DublinSchool of Chemistryp 6 Introduction 1.Introduction to mass spectrometry a- ESI- TOF-MS b- GC- TOF-MS c- LDI-Q-TOF-MS d- ESI-LIT-MS 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries Principle Quadrupole mass analysing device electric field is used to separate ions according to their mass-to-charge ratio as they pass along the central axis of four parallel equidistant metal rods that have fixed (DC) and alternating (RF) voltages. MS n, multiple MS/MS experiments can be done. Sample characteristics Charged or partially charged polar compounds. Sample might need ionisation agent, such as NaCl, Ammonium acetate,... Solvent choice -> see page 7 ESI- LIT-MS Electrospray ionisation coupled to a linear iontrap mass spectrometer References: Lampman GM et al., Spectroscopy, International Edition, 4 th edition. Paul W, Reinhard HP & VonZahn U, 1958., Z. Phys., 152 (2), p API 2000, Applied Biosystems

8 Sample Preparation 1.Introduction to mass spectrometry 2. Sample preparation a- Choice of solvent Sample solubility b- S ample concentration Sample vials 3. Sample submission form 4. Results 5. MS queries Choice of solvent MALDI- QTOF GC-TOF- MS ESI-TOF MeOH, ACN, DCM, CHCl3, EtOAc MeOH, ACN, H2O  H2O, DMSO Sample solubility Sample must be fully dissolved. In the event of partial solubility, filter or centrifuge the sample. Then, decant the supernatant to a clean vial for MS analysis. Trinity College DublinSchool of Chemistryp 7

9 Trinity College DublinSchool of Chemistryp 8 Sample Preparation 1.Introduction to mass spectrometry 2. Sample preparation a- Choice of solvent Sample solubility b- S ample concentration Sample vials 3. Sample submission form 4. Results 5. MS queries Sample concentration Mass Spectrometry is at least 20 times more sensitive than NMR. Do not submit the sample for MS straight from the NMR tube, please. MALDI-QTOF / ESI-TOF GC-TOF-MS ~ 1mg.mL -1 ~ 5mg.mL -1 Sample Vials Use 2 mL HPLC vials with dimension (12 x 32 mm (diameter x height)). Add anything between 0.5 to 1.5 mL solvent but please do not fill to the top of the vial. Things to Avoid in Sample Preparation: - salt buffers such as phosphates, citrates, borates, etc. - detergents - inorganic acids (H2SO4, H2PO4, etc) For HRMS, your sample must be pure.

10 Trinity College DublinSchool of Chemistryp 9 Sample submission form Fill-in where there is a star  Draw the proposed structure, (see example in red) Exact Mass: Formula : C 9 H 16 O Do not forget to indicate the solvent of dilution X XXX 001 YYYY-MM-DD XXX ZZZ X X 1.Introduction to mass spectrometry 2. Sample preparation 3. Sample submission form a- One sample b- More than one sample 4. Results 5. MS queries One sample

11 Trinity College DublinSchool of Chemistryp 10 Sample submission form 1.Introduction to mass spectrometry 2. Sample preparation 3. Sample submission form a- One sample b- More than one sample 4. Results 5. MS queries See Attachment X 4 samples YYYY-MM-DD XXX ZZZ X X More than one sample Exact Mass: Formula : C 9 H 16 O Exact Mass: Formula : C 9 H 16 O Exact Mass: Formula : C 10 H 10 Exact Mass: Formula : C 9 H 16 O XXX 001 XXX 002 XXX 004 XXX 003

12 Trinity College DublinSchool of Chemistryp 11 Results 1.Introduction to mass spectrometry 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries Experimental Mass Theoritical Mass Δm * Mass Accuracy ** Unsaturation degree Isotopic Pattern matching Empirical formula *, |Expected mass – Theoretical mass| * *, [Δm/(integer value of m)]x10 6 Name (Supervisor), XXX 001

13 Trinity College DublinSchool of Chemistryp 12 MS queries 1.Introduction to mass spectrometry 2. Sample preparation 3. Sample submission form 4. Results 5. MS queries Any questions regarding the mass spectrometry service in TCD then please ask Dr. Martin Feeney or Dr. Bernard Jean-Denis.Dr. Martin Feeney Dr. Bernard Jean-Denis The mass spectrometry main lab phone number is If you would like to attend the MS course taught in the Dublin Chemistry programme, please contact Dr. Jimmy Muldoon.Dr. Jimmy Muldoon The course is usually scheduled for January-March of every year. Alternatively check the website:


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