气相色谱-串联质谱法测定生姜中的黄樟素

Determination of Safrole in Ginger by Gas Chromatography-Tandem Mass Spectrometry

摘要:

建立了固相萃取净化结合气相色谱-质谱联用仪测定生姜中的黄樟素的分析方法。实验优化了样品前处理条件和色谱质谱条件。样品经乙腈提取，高速离心后，采用Carb-NH2固相小柱富集净化，洗脱液经旋转蒸发仪浓缩。采用气相色谱分离，多反应离子监测模式（MRM）进行黄樟素质谱检测。以基质匹配标准溶液外标法定量测定。实验结果表明，黄樟素在0.005~0.5 μg/mL范围内呈良好的线性关系，相关系数（R2）大于0.999，方法检出限（S/N=3）为0.42 μg/kg，定量限（S/N=10）为1.41 μg/kg，在5、25、50 μg/kg 3个添加水平下，样品中黄樟素的平均回收率为107.7%~111.9%，相对标准偏差为2.02%~2.32%。该方法具有灵敏度高、富集效果好、回收率高等优点，为生姜及其生姜制品中的黄樟素筛查提供技术支持。用本研究建立的方法检测151个生姜样品，发现部分生姜样品中有微量黄樟素检出，浓度范围为0.45~1.3 μg/kg。

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.