This document discusses the use of surface activated chemical ionization (SACI) coupled with ion exchange chromatography for the analysis of polar low molecular weight drugs like morphine-3-glucoronide and morphine-6-glucoronide. Preliminary experiments showed that SACI produced better signals with less fragmentation compared to atmospheric pressure chemical ionization and electrospray ionization. SACI also showed less signal suppression during chromatographic analysis. The method was applied to urine samples without pre-treatment and showed good separation of analytes and low matrix effects. Future work will involve varying parameters and applying the LC-CEC-SACI-MS method to screen other drug metabolites in biological samples.
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Saci And Ion Exchange Chromatography
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
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)
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
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.
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