固相萃取-气相色谱-质谱法测定植物饮料中的9种植物毒素

Determination of Nine Phytotoxins in Botanical Beverage by Solid-phase Extraction and Gas Chromatography-mass Spectrometry

建立了固相萃取(SPE)净化结合气相色谱-质谱联用(GC-MS)同时检测植物饮料中9种植物毒素(侧柏酮、龙蒿脑、长叶薄荷酮、黄樟素、甲基丁香酚、香豆素、α-细辛脑、β-细辛脑和山道年)的分析方法。样品高速离心后,采用HLB固相萃取小柱富集净化,洗脱液经氮吹浓缩,以DB-5MS色谱柱分离,GC-MS选择离子监测模式测定。实验表明,9种植物毒素在5~1000μg/L浓度范围内线性关系良好,相关系数均大于0.999;方法检出限(S/N=3)为0.3~1.4μg/kg,定量限(S/N=10)为1.0~4.7μg/kg;阴性样品的3个添加水平的平均回收率在76.3%~99.7%之间,相对标准偏差(RSD,n=6)小于8.7%。该方法处理简单,准确高效,适用于植物饮料中9种植物毒素的检测。8个实际样品的检测结果显示,有1个草本饮料样品检出0.7 mg/kg甲基丁香酚。

A sensitive method was established for the simultaneous determination of nine phytotoxins, including thujone, estragole, pulegone, safrole, methyl eugenol, coumarin, santonin, and a-and 13-asarone, in botanical beverage by solid-phase extraction （SPE） and gas chromatography-mass spectrometry （GC-MS）. Samples were extracted and purified using hydrophilic lipophilic balanced （HLB） SPE cartridges after high-speed centrifugation. Finally, the eluent was concentrated by nitrogen gas blowing and all samples were separated using DB-5MS capillary chromatographic column and detected by GC-MS with selected ion monitoring （S/M）. The results indicated good linear relationships in the range of 5-1000 p.g/L for the nine phytotoxins, with correlation coefficient 〉0.999. The limits of detection （LODs, S/N=3） and quantification （LOQs, S/N=10） of the method for the target compounds were in the range of 0.3-1.4 and 1.0~4.7 lag/kg, respectively. The mean recoveries of negative samples at three spiked levels were between 76.3% and 99.7%, and the relative standard deviation （RSD, n=6） was 〈8.7%. This method was suitable for the identification and quantification of nine phytotoxins in botanical beverage owing to its simplicity and accuracy. Among eight actual samples tested, one sample of herb beverage was found containing 0.7 mg/kg methyl eugenol.