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

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


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.


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


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