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Keywords:

  • Atmospheric pressure chemical ionisation-MS;
  • Brassicaceae;
  • desulphoglucosinolates;
  • ESI-MS;
  • HPLC

Abstract

In order to develop a sensitive method for the detection of desulphoglucosinolates by HPLC-MS, the two most common interfaces for HPLC-MS, atmospheric pressure chemical ionisation (APCI) and ESI, were compared. While working with the APCI-interface the evaporation temperature and corona amperage were optimised. In doing so 300°C and 6 μA proved to be most suitable for aliphatic and indole desulphoglucosinolates. The use of formic acid instead of water in the eluent in HPLC-ESI-MS measurements increased the sensitivity for the indole desulphoglucosinolates in the presence of 1 mM formic acid, while the sensitivity for the aliphatic desulphoglucosinolate desulphoglucoraphanin was substantially increased by the presence of 5 mM formic acid. Using an Agilent ion trap, two optimisation procedures for the MS parameters, smart and expert mode, were available. In smart mode the software optimises several parameters automatically, which is much more time efficient than expert mode, in which the optimisation is done manually. It turned out that ESI-MS is most sensitive in smart mode, while for APCI-MS a higher sensitivity could be gained using the expert mode. Comparing both interfaces, APCI-MS was more sensitive than ESI-MS. However, no additional information, in terms of structure determination, was obtained by APCI-MS.