采用二(四氧杂杯[2]芳烃[2]三嗪)固相萃取材料检测果汁中的芦丁

DETERMINATION OF RUTIN IN FRUIT JUICE BY USING BIS(TETRAOXACALIX[2]ARENE[2]TRIAZINE ) AS A SORBENT

通过化学反应,将二（四氧杂杯[2]芳烃[2]三嗪）键合到硅胶表面,制备了一种新型的固相萃取（solid-phase extraction,SPE）材料,并采用红外光谱仪和元素分析仪对合成的固相萃取材料进行了表征。结合高效液相色谱（HPLC）,以芦丁为目标分析物对萃取性能进行了考察,结果表明这种新型的吸附剂可以提供多种分子间作用力,如π-π、疏水和氢键作用等。为了获得最优的固相萃取条件,对影响萃取效率的因素（如上样p H、速率,洗脱剂的种类、体积,淋洗液类型、体积等）进行了优化。在最优化的样品前处理条件下,建立分析方法,并用于果汁样品中芦丁含量的分离分析,结果表明在0.02~1.0μg/m L的范围内线性关系良好,方法的最低检测限是6.5 ng/m L,回收率在94.5%~98.2%之间,相对标准偏差〈3.3%（n=5）。该方法对实际样品进行分析时,灵敏度高、测定结果准确,可用于果汁等样品中芦丁含量的分离分析。

Solid phase extraction（SPE）is widely used in the separation and enrichment of the target analytes in complex matrix. A novel solid-phase extraction（SPE） sorbent was synthesized by chemical immobilization of bis（tetraoxacalix [2]arene [2]triazine） onto pure silica gel in the present study. The bis（tetraoxacalix [2]arene [2]triazine） modified silica gel was evaluated by elemental analysis（EA） and Fourier transform infrared spectroscopy（FT-IR）. The extraction performance of the sorbent was evaluated using rutin as model analyte combined with high performance liquid chromatography（HPLC） analysis. Factors that influence the extraction efficiency including sample solution p H,sample loading rate,eluent type,volume of eluent,elution rate,and volume of sample loading were optimized. The results showed that the new sorbent could offer multiple intermolecular interactions, such as π-π, hydrophobic and hydrogen bonding interactions. The optimum extraction conditions were as follows： sample solution p H of 4;sample loading rate of 1.5 m L/min;eluent type of 5% methanol; eluent volume of 3 m L;elution rate of 0.5 m L/min and sample loading volume of 10 m L.Under the optimal conditions,the proposed method was established and applied for the analysis of rutin in fruit juice. Satisfactory linear range was obtained in the range of 0.02-1.0 μg/m L for rutin with correlation coefficient（R2）of 0.999 8. Limit of detection（LOD）was 6.5 ng/m L,while the recovery rates of rutin ranged from 94.5%to 98.2% with relative standard deviations（RSD） less than 3.3%（n=5）. As a novel solid-phase extraction sorbent,the bis（tetraoxacalix [2]arene [2]triazine）-modified silica exhibited a higher extraction efficiency of the rutin in juice samples.