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Mass Spectrometry II. Ion trap. Magnetic Sector. F B. Magnetic Sector. Magnetic Sector. Ion-source. detector. +. +. +. +. +. +. +. +. Mass is determined by the time it takes the ion to move from source to detector. +. +. +. +. +. +. +. +. +. +. +. +. +. +. +. +.

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Presentation Transcript
slide6

Ion-source

detector

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Mass is determined by the time it takes the ion to move from source to detector

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L (length)

t =

+

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(velocity)

-

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(acceleration voltage)

2V

Field-free flight zone

Acceleration

zone

 =

(m/z)

(mass-to-charge)

Time of Flight MS

In a quadrupole MS masses are separated based on their flight path

In a time-of-flight MS masses are separated based on their inertia

slide7

301.14 to 301.16 amu

169.09 to 169.08 amu

179.10 to 179.12 amu

193.12 to 193.14 amu

281.13 to 281.15 amu

235.16 to 235.19 amu

slide9

MS Application

  • Environmental Issue:
    • Presence of bioloigcally-active compounds (pharmaceuticals…) that are not degraded in a wastewater treatment plant
    • Compound of interest is trimethoprim, an anti-microbial used to treat infectious diseases in humans
  • Analytical - want to analyze for trimethoprim
    • LC/GC?
  • Ionization source?

LC – why?

ESI – why?

  • Hypothesis
    • Primary treatment of wastewater with nitrifying activated sludge will degrade trimethoprim
slide10

MS Application

  • Hypothesis
    • Primary treatment of wastewater with nitrifying activated sludge will degrade trimethoprim
  • Experiment
    • Small scale laboratory batch reactor was used to degrade trimethoprim
    • LC-ESI coupled to a single quadrupole MS to determine the unit mass of degradation products
    • LC-ESI coupled to an ion trap MS to determine structural features of the degradation products
    • LC-ESI coupled to a quadrupole time of flight MS to determine the accurate mass of the degradation products to get a chemical formula
slide11

MS Application

  • Hypothesis
    • Primary treatment of wastewater with nitrifying activated sludge will degrade trimethoprim
  • Experiment
    • Small scale laboratory batch reactor was used to degrade trimethoprim
    • LC-ESI coupled to a single quadrupole MS to determine the unit mass of degradation products
    • LC-ESI coupled to an ion trap MS to determine structural features of the degradation products
    • LC-ESI coupled to a quadrupole time of flight MS to determine the accurate mass of the degradation products to get a chemical formula
slide12

MS Application

Data from

LC-ESI-single quad MS

MW: 290.32 g mol-1

Total ion chromatogram

Degradation products

Parent [M+1]

Single ion chromatogram

Anything strange…

slide13

MS Application

  • Experiment
    • LC-ESI coupled to a single quadrupole MS to determine the unit mass of degradation products
      • 2 degradation products
      • [M+H] of 307 m/z and 325 m/z
      • Increased mass but earlier LC elution
      • Suggests oxidation
        • Mass difference between 291 m/z and 307 m/z is 16 m/z (oxygen)
        • Mass difference between 291 m/z and 325 m/z is 34 m/z (2O and 2 H)
slide14

MS Application

Data from

LC-ESI-Ion trap MS (MS2)

LC mobile phase is H2O and CH3OH

291 (trimethoprim) trapped in ion trap

Accelerated/dissociated and the products detected

[M+H] is 291

291 m/z → products

slide15

MS Applications

  • Experiment
    • LC-ESI coupled to a single quadrupole MS to determine the unit mass of degradation products
      • 2 degradation products
      • [M+H] of 307 m/z and 325 m/z
      • Increased mass but earlier LC elution
      • Suggests oxidation
        • Mass difference between 291 m/z and 307 m/z is 16 m/z (oxygen)
        • Mass difference between 291 m/z and 325 m/z is 34 m/z
  • LC-ESI coupled to an ion trap MS to determine structural features of the degradation products
    • Parent
    • Demonstrates that the phenyl rings are recalcitrant to dissociation
    • Useful information for the ion trap analysis of the degradation products
slide16

MS Application

Data from

LC-ESI-Ion trap MS (MS2)

307-18

Loss of water

[M + H – H2O]+

Degradation product 307 m/z trapped in ion trap Accelerated/dissociated and the products detected

307 m/z → products

D2O and CD3OD

slide17

MS Application

Data from

LC-ESI-Ion trap MS (MS3)

Degradation product 307 m/z trapped in ion trap Accelerated/dissociated and 289 m/z trapped in ion trap

Accelerated/dissociated and the products detected

Can be formed from the dissociation of 307m/z or 289 m/z

307 m/z → 289 m/z → products

D2O and CD3OD

slide18

MS Application

Data from

LC-ESI-Ion trap MS (MS3)

Degradation product 307 m/z trapped in ion trap Accelerated/dissociated and 274 m/z trapped in ion trap

Accelerated/dissociated and the products detected

Can be formed from the dissociation of 289 m/z and 274 m/z

307 m/z → 274 m/z → products

D2O and CD3OD

slide19

MS Application

  • Experiment
    • LC-ESI coupled to a single quadrupole MS to determine the unit mass of degradation products
      • 2 degradation products
      • [M+H] of 307 m/z and 325 m/z
      • Increased mass but earlier LC elution
      • Suggests oxidation
        • Mass difference between 291 m/z and 307 m/z is 16 m/z (oxygen)
        • Mass difference between 291 m/z and 325 m/z is 34 m/z
  • LC-ESI coupled to an ion trap MS to determine structural features of the degradation products
    • Parent
    • Demonstrates that the phenyl rings are recalcitrant to dissociation
    • Useful information for the ion trap analysis of the degradation products
  • Products
  • Use MS3 data to propose a fragmentation pathway for 307 m/z degradation product
  • Structure confirmation
slide20

MS Application

Data from

LC-ESI-Ion trap MS (MS2 and MS3)

Propose fragment structures

- H, - OH, - CH3

slide21

MS Application

  • Experiment
    • Small scale laboratory batch reactor was used to degrade trimethoprim
    • LC-ESI coupled to a single quadrupole MS to determine the unit mass of degradation products
    • LC-ESI coupled to an ion trap MS to determine structural features of the degradation products
    • LC-ESI coupled to a quadrupole time of flight MS to determine the accurate mass of the degradation products to get a chemical formula
  • Hypothesis
    • Primary treatment of wastewater with nitrifying activated sludge will degrade trimethoprim
  • Answer
    • Degradation of trimethoprim is possible using nitrifying activated sludge
    • Degradation products identified using several MS techniques
slide22

MS Application

Data from

LC-ESI-Ion trap MS

LC mobile phase is D2O and CD3OD

296 (d-trimethoprim) trapped in ion trap

Accelerated/dissociated and the products detected

[M+D] is 296

slide23

MS Application

Data from

LC-ESI-Ion trap MS

H2O and CH3OH

D2O and CD3OD