改进QuEChERS-气相色谱-质谱法快速分析蜂花粉中的多环芳烃

Rapid Determination of Polycyclic Aromatic Hydrocarbons in Bee Pollen by GC-MS Coupled with Modified Qu ECh ERS

建立了蜂花粉中16种多环芳烃（PAHs）的QuEChERS快速提取、净化方法及气相色谱-质谱检测方法。蜂花粉样品经水溶解后在无缓冲体系下用乙腈萃取目标化合物,选择150 mg PSA/150 mg C18/900 mg Mg SO4/500 mg Florisil组合填料进行净化,之后,用GC-MS测定。在最优化色谱条件下,16种PAHs呈现良好的线性关系,方法检出限为0.2～3.3 ng/g,定量限为0.7～11.0 ng/g。大部分PAHs的回收率在61.0%～135.4%之间,相对标准偏差小于11.8%。改进的QuEChERS-GC/MS方法成功应用于蜂花粉（采自不同污染程度地区）PAHs的测定,结果显示不同花粉样品中PAHs种类和含量存在明显差异。本研究为蜂花粉的质量安全评价以及进一步开展蜂花粉与环境污染物之间相关性研究奠定了基础。

A rapid analytical method based on modified QuEChERS sample preparation and GC-MS for the analysis of 16 polycyclic aromatic hydrocarbons（PAHs） in bee pollen has been developed. Bee pollen samples were firstly dissolved in water, the targeted compounds were extracted with acetonitrile solution under the no buffer system conditions and purified with 150 mg PSA/150 mg C18/ 900 mg Mg SO4/ 500 mg Florisil packing powder,and finally, 16 PAHs were analysed by GC-MS. Under the optimal conditions, the results showed good linearity（R 0.99）, the detection limits of PAHs were between 0.2-3.3 ng/g, and the quantitative limits ranged from 0.7 ng/g to 11.0 ng/g,the average recoveries of most PAHs were in the range of 61.0%-135.4%, the relative standard deviations（RSDs） were below than 11.8%. The modified QuEChERS-GC/MS method was successfully applied to detect PAHs in bee pollen samples collected from different pollution areas,the results showed the difference of sorts and contents of PAHs in the bee pollen samples was evident. The study lay a foundation for the quality and safety evaluation of bee pollen as well as further study on the correlation between bee products and environmental pollutants.