Saci And Ion Exchange Chromatography
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Saci And Ion Exchange Chromatography

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SACI is the only ionization source able to work with ion exchange chromatography. Here an applications is shown.

SACI is the only ionization source able to work with ion exchange chromatography. Here an applications is shown.

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  • 1. Ion exchange chromatography coupled to SACI for the analysis of high polar low molecular weight drugs Sara Crotti, ISB srl XIV Discussion group on Mass Spectrometry
  • 2. Surface Activated Chemical Ionization
  • 3. Ion Exchange Chromatography (IEC)
    • Elution by means of salt of pH gradient
    • For high polar compounds
    Time Ionic strength
  • 4. IEC coupled to Mass Spectrometry: SACI No discharge phenomena (low voltage source) Few application because of analyte degradation and ion suppression phenomena Never applied till now  ESI & APCI Discharge phenomena for the high voltages in API sources
  • 5. Aim: IEC Analysis of M3G and M6G Optimal source: APCI, ESI or SACI? Morphine 3-glucoronide (M3G) Morphine 6-glucoronide (M6G)
  • 6. Preliminary infusion of M3G 50ng/ml: APCI In source fragmentation MW 461 MW 285 0 2.0 3.0 4.0 5 x10 5 150 200 250 300 350 400 450 500 550 m/z 286 1.0 Morphine-3- Glucuronide in source fragment Intensity (counts/s) ‏
  • 7. Preliminary infusion of M3G 50ng/ml: ESI Intensity (counts/s) ‏ 462 3.0 4.0 5.0 6 x10 5 2.0 1.0 0 150 200 250 350 400 450 550 m/z 300 500 [M+H] + Source noise
  • 8. Preliminary infusion of M3G 50ng/ml: Intensity (counts/s) SACI 0.0 2.0 4.0 6.0 x10 5 150 200 250 300 350 400 450 500 550 m/z 462 286 8 Morphine-3- Glucuronide in source fragment [M+H] +
  • 9. M3G and M6G separation with a linear gradient 5-100% B A : H 2 O B : H 2 O + 0.5% formic ac. + 10mM ammonium acetate SACI ESI Cation Exchange Chromatography (CEC) Injection of 500pg Chromatographic analysis:
  • 10. Intensitiy (counts/s) Results : SACI ESI Signal suppression (in source current ~ 40000nA) Good signal (in source current ~ 2 4nA) ‏ 2 4 6 8 10 12 Time [min] 0 200 400 600 800 Intensitiy (counts/s) ‏ 2 4 6 8 10 12 Time [min] 0.0 0.5 1.0 1.5 2.0 5 x10 10.11 8.42 Morphine-6- Glucuronide Morphine-3- Glucuronide
  • 11. SACI urine sample analysis: Urine sample Dil. 1:5 In H 2 0 10  l inj 2 4 6 8 10 12 Time [min] 0.0 0.5 1.0 1.5 2.0 x10 5 10.15 8.48 M3G M6G Intensitiy EIC m/z 462 m/z 286
  • 12. Matrix effect: 20 negative urine spiked vs Standard solution % Var= (Au-As)/As*100 sample %Area variation urine vs Water samples 1 -6 2 -8 3 -6 4 -1 5 -5 6 -7 7 -4 8 -4 9 -5 10 -5 11 -5 12 -5 13 -0,5 14 -2 15 -1 16 -1 17 -4 18 -3 19 -3 20 -2
  • 13. Conclusions:
    • SACI is the only source suitable to coupling ion exchange chromatography with mass spectrometry
    • Analysis in urine is performed by SACI without any sample pre-tratment tanks to a low matrix effect
    • Good separation of analytes obtained with CEC
  • 14. Future steps: Next experiments with potential and salt concentration variation Application of LC-CEC-SACI-MS for screening of other addictive drug metabolites in biological sample.
  • 15. Where do you can find us ? Web site: http://www.isbiotechnology.com