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A Dedicated Mass Spectrometer Tuning Method for SFC–MS and Evaluation of Two Different Linear Restrictor Types Used in the Operation of a Split Flow Pre-Back Pressure Regulator SFC–MS Interface

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Abstract

The operation of a SFC–MS system has been improved. The SFC–MS interface uses a post-column make-up flow of liquid whose supply line to the SFC–MS interface mixing tee is equipped with an injection valve. Prior to analysis, this arrangement permits a stable flow of a dilute tune solution of analyte(s) for the exact amount of time required to optimize mass spectrometry tuning. Advantageously, with this arrangement tuning is performed in the presence of the exact split flow and same composition of SFC mobile phase and make-up liquid to be used for subsequent SFC–MS operation. The SFC–MS interface was constructed to provide a pre-back pressure regulator split flow to the mass spectrometer using a linear restrictor. Two different linear restrictors constructed from either 50 µm i.d. PEEK tubing or 25 µm i.d. fused silica tubing were evaluated. For best electrospray performance, each restrictor required a different post-column make-up flow rate. The use of either restrictor retained a high degree of chromatographic fidelity for the SFC separation of six pharmaceutical compounds using a cyanopropyl column with a mobile phase of supercritical fluid carbon dioxide modified with methanol and aqueous ammonia solution. Each restrictor provided a different level of SFC–MS performance for each of the six pharmaceutical compounds tested. Based upon overall performance, a linear fused silica restrictor was selected to develop a chromatographic separation using on-line SFC–MS for three structurally very similar monensin sodium salt analogues that are not directly amenable to off-line SFC using UV/Vis detection.

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References

  1. Smith RD, Fjeldsted J, Lee ML (1983) Int J Mass Spectrom Ion Phys 46:217–220

    Article  CAS  Google Scholar 

  2. Combs MT, Ashraf-Khorassani M, Taylor LT (1997) J Chromatogr A 785:85–100

    Article  CAS  Google Scholar 

  3. Matsumoto K (1994) Org Mass Spectrom 29:266–268

    Article  CAS  Google Scholar 

  4. Sadoun F, Virelizier H, Arpino PJ (1993) J Chromatogr A 647:351–359

    Article  CAS  Google Scholar 

  5. Moyano E, McCullagh M, Galcerana MT, Games DE (1997) J Chromatogr A 777:167–176

    Article  CAS  Google Scholar 

  6. Carrott MJ, Jones DC, Davidson G (1998) Analyst 123:1827–1833

    Article  CAS  Google Scholar 

  7. Garzotti M, Rovatti L, Hamdan M (2001) Rapid Commun Mass Spectrom 15:1187–1190

    Article  CAS  PubMed  Google Scholar 

  8. Berger TA, Berger BK, Majors RE (2010) LC-GC North Am 28:344–357

    CAS  Google Scholar 

  9. Pinkston JD, Wen D, Morand KL, Tirey DA, Stanton DT (2006) Anal Chem 78:7467–7472

    Article  CAS  PubMed  Google Scholar 

  10. Desfontaine V, Guillarme D, Francotte E, Novakova L (2015) J Pharm Biomed Anal 113:56–71

    Article  CAS  PubMed  Google Scholar 

  11. Berger TA, Berger BK (2013) Chromatographia 76:591–601

    Article  CAS  Google Scholar 

  12. Taylor LT (2009) J Supercrit Fluids 47:566–573

    Article  CAS  Google Scholar 

  13. Poole CF (2012) J Chromatogr A 1250:157–171

    Article  CAS  PubMed  Google Scholar 

  14. Lemasson E, Bertin S, West C (2016) J Sep Sci 39:212–233

    Article  CAS  PubMed  Google Scholar 

  15. Grand-Guillaume Perrenoud A, Veuthey JL, Guillarme D (2014) Trac Trends Anal Chem 64:44–55

    Article  CAS  Google Scholar 

  16. Taylor LT (2012) J Chromatogr A 1250:196–204

    Article  CAS  PubMed  Google Scholar 

  17. Cazenave-Gassiot A, Boughtflower R, Caldwell J, Hitzel L, Holyoak C, Lane S, Oakley P, Pullen F, Richardson S, Langley GJ (2009) J Chromatogr A 1216:6441–6450

    Article  CAS  PubMed  Google Scholar 

  18. Desfontaine V, Veuthey JL, Guillarme D (2017) Hyphenated detectors: mass spectrometry. In: Poole CF (ed) Supercritical fluid chromatography. Elsevier, Amsterdam

    Google Scholar 

  19. Guillarme D, Desfontaine V, Heinisch S, Veuthey JL (2018) J Chromatogr B 1083:160–170

    Article  CAS  Google Scholar 

  20. Novakova L, Grand-Guillaume Perrenoud A, Nicoli R, Saugy M, Veuthey JL, Guillarme D (2015) Anal Chim Acta 853:637–646

    Article  CAS  PubMed  Google Scholar 

  21. Grand-Guillaume Perrenoud A, Veuthey JL, Guillarme D (2014) J Chromatogr A 1339:174–184

    Article  CAS  Google Scholar 

  22. Fujito Y, Hayakawa Y, Izumi Y, Bamba T (2017) J Chromatogr A 1508:138–147

    Article  CAS  PubMed  Google Scholar 

  23. Moran JW, Rodewald JM, Donoho AL, Coleman MR (1994) J AOAC Int 77:885–890

    CAS  PubMed  Google Scholar 

  24. Berry AJ, Ramsey ED, Newby M, Games DE (1996) J Chromatogr Sci 34:245–253

    Article  CAS  Google Scholar 

  25. Li B, Guo W, Song W, Ramsey ED (2016) J Supercrit Fluids 115:17–25

    Article  CAS  Google Scholar 

  26. Ramsey ED, Berry AJ, Lawrence SD, Games DE, Startin JR (1995) Rapid Commun Mass Spectrom 9:712–716

    Article  CAS  Google Scholar 

  27. Ramsey ED, Rees AT, Wei G, Liu JY, Wu XH (2010) J Chromatogr A 1217:3348–3356

    Article  CAS  PubMed  Google Scholar 

  28. Li B, Guo W, Chi HJ, Kimura M, Ramsey ED (2017) Chromatographia 80:1179–1188

    Article  CAS  Google Scholar 

  29. Li B, Guo W, Ramsey ED (2018) J Supercrit Fluids 133:372–382

    Article  CAS  Google Scholar 

Download references

Acknowledgements

Edward D. Ramsey wishes to express his sincere gratitude for the financial support provided by the Chinese Central Government for Foreign Experts in the framework of the 1000 Plan Program (WQ2012210006) and also for Grant GDW20172100109 to support this study.

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Authors and Affiliations

  1. Sustainable Technology Research Centre, University of Science and Technology Liaoning, 185 Qianshan Road, Anshan, 114051, China

    Wei Guo, Ben Li, Haijun Chi & Edward D. Ramsey

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  1. Wei Guo
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  2. Ben Li
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  3. Haijun Chi
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  4. Edward D. Ramsey
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Correspondence to Edward D. Ramsey.

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Guo, W., Li, B., Chi, H. et al. A Dedicated Mass Spectrometer Tuning Method for SFC–MS and Evaluation of Two Different Linear Restrictor Types Used in the Operation of a Split Flow Pre-Back Pressure Regulator SFC–MS Interface. Chromatographia 81, 1257–1267 (2018). https://doi.org/10.1007/s10337-018-3565-6

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  • DOI: https://doi.org/10.1007/s10337-018-3565-6

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