咪唑类离子液体-β-环糊精聚合物固相萃取-紫外分光光度法测定药品和食品中芦丁

UV-Spectrophotometric Determination of Rutin in Medicine and Food Products with Separation by SPE Using Ionic Liquid Loaded β-Cyclodextrin Cross-Linked Polymer as Solid Extractant

以自制的咪唑类离子液体-β-环糊精聚合物(IL-β-CDCP)作为萃取剂,对药品和食品中芦丁的固相萃取(SPE)分离条件进行了优化,并用紫外分光光度法测定样品中芦丁的含量。结果表明:在含芦丁的pH 4.0乙酸盐缓冲溶液40mL中加入IL-β-CDCP 0.1g,于15.0℃水浴中振荡10.0min后,可使92.0%的芦丁吸附在IL-β-CDCP上。离心分离后,吸附了芦丁的IL-β-CDCP留在下层。将其分出并在其中加无水乙醇4.0mL,于35.0℃水浴振荡10.0min,可使芦丁从IL-β-CDCP洗脱,溶入于乙醇中,脱附率达94.0%,于360nm处测量洗脱液的吸光度。芦丁的质量浓度在0.06~7.0mg·L^(-1)内与其吸光度呈线性关系,检出限(3s/k)为8.1μg·L^(-1)。测定值的相对标准偏差(n=6)为0.38%~1.7%。

Self-prepared cross-linked polymer formed between imidazole ionic liquid andβ-cyclodextrin（IL-β-CDCP）was used as solid extractant in the SPE of rutin from samples of medicine and food,and optimum conditions for the separation were studied.The analyte（rutin）was then determined by UV-spectrophotometry.As shown by the results,when 0.1g of IL-β-CDCP was added to 40 mL of acetate buffer solution（pH 4.0）containing rutin,and the mixture was shaked for 10.0min in a water bath heated at 15.0 ℃,92.0% of the rutin was found adsorbed on IL-β-CDCP.After centrifugation,and removing the super liquid phase,absolute alcohol（4.0mL）was added to the IL-β-CDCP adsorbed with rutin settled in the lower phase,and the mixture was shaked for 10.0min at 35.0℃in a water bath,during which 94.0% of the adsorbed rutin was eluted from IL-β-CDCP and dissolved in alcohol.The absorbance of the alcohol solution was measured at 360 nm.Linear relationship between values of absorbance and mass concentration of rutin was found in the range of 0.06 to 7.0mg·L^（-1）,with detection limit（3s/k）of 8.1μg·L^（-1）.Values of RSD′s（n=6）found were range from 0.38% to 1.7%.