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A Combined Electrospray and APCI ionization system Peter Kovarik and Yves LeBlanc

A Combined Electrospray and APCI ionization system Peter Kovarik and Yves LeBlanc system offers simultaneous operation of Electrospray and APCI or software controlled selection of the ionization process allowing a rapid transition between the two techniques. Dual Source “Duo”.

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A Combined Electrospray and APCI ionization system Peter Kovarik and Yves LeBlanc

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  1. A Combined Electrospray and APCI ionization system Peter Kovarik and Yves LeBlanc system offers simultaneous operation of Electrospray and APCI or software controlled selection of the ionization process allowing a rapid transition between the two techniques

  2. Dual Source “Duo” Turbo “V” Source

  3. Applications of Dual Source • quantitative applications: • 1. method development (choosing the best ionization mode) • 2. multiple ionization modes in a single run for multiple • components. • B. qualitative applications: • 1. alternate full scan APCI/ESI for spectra interpretation

  4. 4.0e4 Mometasone 3.6e4 Minoxidil APCI TIS Intensity, cps Intensity, cps Minoxidil Mometasone 0.0 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 0.5 1.0 1.5 2.0 2.5 3.0 3.5 Time, min Time, min Two period experiment: 0-2.1 minutes TIS, 2.2-4.0 minutes APCI 4.4e4 TIS APCI Minoxidil Mometasone Intensity, cps 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 Time, min

  5. Ion suppression – comparison of TIS and APCI post column split infusion introduced a steady flow of Minoxidil into the source, blank urine sample was then injected onto the column and variation in the MRM signal was monitored APCI shows a lower susceptibility to matrix suppression 100% red trace is APCI blue trace is TIS Relative Intensity 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 Time, min

  6. Complementary information offered by the APCI/ESI response 240.2 255.2 2e5cps 220.2 245.1 Ritalinic acid, M+H red trace is APCI 265.1 no M-H 329.1 red trace is APCI 242.2 371.2 200 600 100% 100% 100% 297.0 M+H 1e6cps 220.2 blue trace is TIS M+Na 242.2 313.1 Relative Intensity Relative Intensity Relative Intensity Salicyl acyl Glucuronide M-H 245.1 blue trace is TIS Relative Intensity 287.1 264.0 329.2 369.2 0.0 0.0 0.0 240 240 250 250 260 260 270 270 280 280 290 290 300 300 310 310 320 320 330 330 505.4 255.2 321.1 265.1 200 600 m/z, amu m/z, amu

  7. Performance comparison with a Turbo V source Sensitivity: Reserpine by ESI based TurboIonSpray ( at 0.2mL/min) normalized peak height is ~0.8 of the dedicated source normalized S/N is ~0.5 of the dedicated source Reserpine by APCI ( at 1mL/min) normalized peak height is ~0.6 of the dedicated source normalized S/N is ~0.6 of the dedicated source Background: similar performance to a dedicated source Stability: similar performance to a dedicated source

  8. Examples: A. Gemcitabine and its metabolite highlights the search for maximum sensitivity with ionization switching in a single LC run B. Detection of Salicyl Acyl Glucuronide is an example of a qualitative application that uses fast switching for confirmation of compound structure

  9. MRM analysis of Gemcitabine and it’s metabolite two period experiment sets an optimum ionization, ion polarity and desolvation temperature for each compound compounds and LC conditions were provided by Dr. Fabio Garofolo (LLBR – Eli Lilly Canada Inc.) 100% switch APCI positive ion mode T=450C TIS negative ion mode T=550C Relative Intensity metabolite Gemcitabine & metabolite Parent drug 1.0 2.0 3.0 4.0 5.0 0 further results presented as poster #308 (Wed) Time, min

  10. 313 313 137 salicylic acid MW 138 Da COOH 174.8 174.7 OH 137 Relative Intensity 113 269 295 113 285 100 200 300 100 200 300 m/z, amu m/z, amu salicyl glucuronide MW 314 Da salicyl acyl glucuronide MW 314 Da 1 2 3 4 5 6 7 8 9 10 0 Time, min Identification of salicylic acid glucuronide metabolites neutral loss experiment (loss of 176amu) 100% Blue trace – TIS Red trace - APCI

  11. Confirmation of thermally decomposing glucuronide TIC - neutral loss of 176 amu Blue trace – TIS Red trace - APCI Intensity 1 2 3 4 5 6 7 8 9 10 Time, min Extracted mass 313 amu Blue trace – TIS Red trace - APCI salicylic acid MW 138 Da COOH Intensity OH 1 2 3 4 5 Time, min red trace – APCI Q1 scan – extracted mass 137 amu blue trace – TIS Q1 scan – extracted mass 313 amu salicyl glucuronide MW 314 Da salicyl acyl glucuronide MW 314 Da Intensity 1 2 3 4 5 6 7 8 9 Time, min

  12. Summary: -Combined ionization source offers an expanded compound class coverage over single mode sources -Duo source allows fast empirical determination and selection of best ionization for compound detection -Qualitative applications offer an advantage in spectra interpretation through identification of adducts and through structural confirmation of thermally labile compounds Acknowledgments: Takeo Sakuma, Stan Potyrala and Toha Dang

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