Determination of Safrole in Ginger by Gas Chromatography-Tandem Mass Spectrometry
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Abstract:
An analytical method for the determination of safrole in ginger by solid-phase purification combined with gas chromatography-mass spectrometry was developed. The conditions of sample pretreatment and analysis by chromatographic mass spectrometry were optimized. The samples were extracted with acetonitrile, centrifuged at a high speed, and then enriched and purified by a Carb-NH2 solid-phase cartridge. The eluate was concentrated by a rotary evaporator. Gas chromatographic separation and multiple reactive ion monitoring mode (MRM) were applied to determine safrole. The matrix-matched external calibration involving standard solutions was used for quantitative analysis. The experimental results show that safrole exhbited a good linear relationship in the range of 0.005~0.5 μg/mL, with the correlation coefficient (R2) higher than 0.999, the limit of detection (S/N=3) as 0.42 μg/kg, and the limit of quantification (S/N=10) as 1.41 μg/kg. The average recoveries of the samples spiked with safrole standard at 5, 25 and 50 μg/kg were 107.7%~111.9%, with the relative standard deviations (RSDs) in the range of 2.02%~2.32%. This method has the advantages of high sensitivity, good enrichment and high recovery rate, and provide technical support for the screening of safrole in ginger and its derived products. Using the developed method, a trace amount of safrole was detected (concentration: 0.45~1.3 μg/kg) in 151 ginger samples.