Determination of Higenamine in Spices by High Performance Liquid Thromatography-Tandem Mass Spectrometry
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Abstract:
A rapid analytical method for determination of higenamine in spices had been developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) in this work. The sample pretreatment conditions and the HPLC-MS/MS conditions were optimized. The sample was extracted with 80% methanol water by volume, and then diluted with pure water for a certain number of times. The target compound was separated on a Waters XBridge C18 (150 mm×2.1 mm, 5 μm) column, and determined using electrospray ionization (ESI) source in positive mode with the multiple reaction monitoring (MRM) acquisition mode. It was quantified with the matrix-matched external standard method, which was performed to accurately quantify higenamine in spices. The results showed that this method exhibited a good linearity in the range of 0.05~20.0 ng/mL, with the correlation coefficients (r) of 0.9999. The limit of detetion (LOD, S/N=3) were 0.7 μg/kg, and the limit of quantitation (LOQ, S/N=10) were 2.33 μg/kg. At the three spiked levels, the average recoveries of star anise were in the range of 91.80%~99.97% with the relative standard deviations of 1.43%~2.35%. The method is simple, sensitive, accurate, stable and suitable for the rapid determination of higenamine in spices.
