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Identification of Pitfalls Related to the Analysis of Liquid Chromatography-Tandem Mass Spectrometry and Liquid Chromatography-Time of Flight Mass Spectrometry

액체크로마토그래프-질량분석기를 이용한 정성 및 정량 오류의 확인

Kwon, Jin-Wook;Cho, Yoon-Jae;Rhee, Gyu-Seek
권진욱;조윤제;이규식

  • Received : 2015.01.21
  • Accepted : 2015.09.10
  • Published : 2015.09.30

Abstract

BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

Keywords

Cross-talk;Inaccuracy;LC/MS/MS;Selective reaction monitoring (SRM)

References

  1. Anastassiades, M., Lehotay, S. J., Stajnbaher, D., & Schenck, F. J. (2003). Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce. Journal of AOAC International, 86(2), 412-431.
  2. Antignac, J. P., de Wasch, K., Monteau, F., De Brabander, H., Andre, F., & Le Bizec, B. (2005). The ion suppression phenomenon in liquid chromatography-mass spectrometry and its consequences in the field of residue analysis. Analytica Chimica Acta, 529(1), 129-136. https://doi.org/10.1016/j.aca.2004.08.055
  3. Berg, T., & Strand, D. H. (2011). $^{13}C$ labelled internal standards-A solution to minimize ion suppression effects in liquid chromatography-tandem mass spectrometry analyses of drugs in biological samples?. Journal of Chromatography A, 1218(52), 9366-9374. https://doi.org/10.1016/j.chroma.2011.10.081
  4. Ferrer, I., & Thurman, E. M. (2009). Liquid chromatography-Time of Flight Mass Spectrometry: Principles, Tools and Applications for Accurate Mass Analysis. New York, NJ: Wiley, ISBN 978-0-470-13797-0.
  5. Gosetti, F., Mazzucco, E., Zampieri, D., & Gennaro, M. C. (2010). Signal suppression/enhancement in high-performance liquid chromatography tandem mass spectrometry. Journal of Chromatography A, 1217(25), 3929-3937. https://doi.org/10.1016/j.chroma.2009.11.060
  6. Hughes, N. C., Wong, E. Y., Fan, J., & Bajaj, N. (2007). Determination of carryover and contamination for mass spectrometry-based chromatographic assays. The AAPS Journal, 9(3), E353-E360. https://doi.org/10.1208/aapsj0903042
  7. Nischwitz, V., & Pergantis, S. A. (2006). Optimisation of an HPLC selected reaction monitoring electrospray tandem mass spectrometry method for the detection of 50 arsenic species. Journal of Analytical Atomic Spectrometry, 21(11), 1277-1286. https://doi.org/10.1039/b607535e
  8. Savitzky, A., & Golay, M. J. (1964). Smoothing and differentiation of data by simplified least squares procedures. Analytical Chemistry, 36(8), 1627-1639. https://doi.org/10.1021/ac60214a047
  9. Song, F. (2011). "Cross-Talk" in Scheduled Multiple Reaction Monitoring Caused by In-Source Fragmentation in Herbicide Screening with Liquid Chromatography Electrospray Tandem Mass Spectrometry. Journal of Agricultural and Food Chemistry, 59(9), 4361-4364. https://doi.org/10.1021/jf200592n
  10. Van Eeckhaut, A., Lanckmans, K., Sarre, S., Smolders, I., & Michotte, Y. (2009). Validation of bioanalytical LC-MS/MS assays: evaluation of matrix effects. Journal of Chromatography B, 877(23), 2198-2207. https://doi.org/10.1016/j.jchromb.2009.01.003
  11. Wang, S., Cyronak, M., & Yang, E. (2007). Does a stable isotopically labeled internal standard always correct analyte response?: A matrix effect study on a LC/MS/MS method for the determination of carvedilol enantiomers in human plasma. Journal of Pharmaceutical and Biomedical Analysis, 43(2), 701-707. https://doi.org/10.1016/j.jpba.2006.08.010

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