Biogenic amines (BA) have been extensively studied in recent years due to their potential toxicity and possible use as chemical markers for assessing food quality and in cancer research. The BA were determined in 62 foods commonly consumed in Malaysia. Three sorbent materials; A18C6-MS, DA18C6-MS and AB18C6-MS were also prepared by the chemical immobilization of the crown ether ligands onto mesoporous silica support. The sorbents have been evaluated for the extraction of five BA (TRP, PUT, HIS, TYR, SPD) by the batch sorption and column method. Results obtained showed that all the sorbents exhibit highest selectively towards SPD compared to other BA. AB18C6-MS offers the higher extraction of SPD in the presence of other BA. The applicability of the proposed method for the selective extraction of SPD was demonstrated by the reasonable recoveries attained from both methods (71.2-99.8 %). Miniaturized sample preparation technique based on hollow fiber LPME with in situ derivatization using dansyl chloride also has been successfully developed for the determination of BA in foods. Under the optimized conditions, enrichment factors from 47 to 456 was achieved.