UHPLC-MS/MS Determination of 4-Hexylresorcinol in Shrimps with Solid Phase Extraction

UHPLC-MS/MS was applied to the determination of 4-hexylresorcinol in shrimps with solid phase extraction. Homogenized pulp (5.00 g) of the sample was extracted twice with methanol (10 mL each). 5 mL of the combined extract was taken,and then made up to 10 mL with water. The solution was purified by passing through PRIME HLB SPE column,and then eluted with 4 mL of mixture of methanol and acetonitrile (9+1) containing 1% (mass fraction) ammonia. The eluate was evaporated to near dryness by N₂-blowing at 40℃ in the water bath.The residue was taken up with 1 mL of acetonitrile (6+4) solution. Waters Acquity UPLC BEH C₁₈ chromatographic column was used as stationary phase, and the mixture of acetonitrile and water mixed in different ratios was used as mobile phase in gradient elution. ESI^- and multi-reactions monitor mode were adopted in MS/MS. Linear relationship between values of peak area and mass concentration of 4-hexylresorcinol was kept in the range of 1.0-100.0 μg·L^-1, with detection limit (3S/N) of 0.25 μg·kg^-1. On the base of blank sample, test for recovery was made by standard addition method. Values of recovery found were in the range of 70.1%-88.6%, with RSD's (n=6) in the range of 3.8%-6.4%.