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A novel on-column sequential preconcentration method of field-amplified sample injection induced by acetonitrile coupled with acid stacking-transient isotachophoresis (FASI-AStITP) is developed for simply but efficiently concentrating alkaloid cations in high-salt sample matrix in capillary electrophoresis (CE).The addition of 70% acetonitrile in sample solution with high-salt sample matrix not only induces field-amplified sample stacking by decreasing conductivity but acts as termination reagent in the succedent tITP.After sample injection completed, a plug of H+ was injected electrokinetically and a neutralization reaction between H+ and tartrate from the buffer solution produced a low conductivity zone, in which the injected analyte cations were further concentrated.