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    超声萃取-流动注射液滴荧光增敏法测定苦荞中芦丁

    Determination of Rutin in Tartary Buckwheat by Ultrasonic Extraction Combined with Flow-Injection Liquid Drops Spectrofluorimetry

    • 摘要: 基于Al3+-芦丁形成络合物的荧光增敏特性,建立了超声萃取-流动注射液滴荧光增敏法测定苦荞中芦丁含量的方法。称取2.000 0 g样品,加入10 mL甲醇并搅拌均匀,超声振荡萃取15 min,以6 000 r·min-1转速离心5 min后移出上层清液,重复此操作2次后合并3份上清液,旋转蒸发除去甲醇溶剂,用90%(体积分数)乙醇溶液溶解,过滤,加入0.1 mol·L-1 Al (NO33溶液5 μL后定容至10.0 mL,静置60~70 min。流动注射速率保持4~5 mL·h-1,激发和发射波长分别为239,507 nm时测定荧光强度。Al3+与芦丁的络合比为1:2,Al3+-芦丁络合物的质量浓度与其荧光强度在0.10~5.00 mg·L-1内呈线性关系,检出限(3s)为0.02 mg·L-1,回收率在86.0%~104%之间,测定值的相对标准偏差(n=5)在3.1%~6.1%之间。方法适合于苦荞中芦丁的常规检测。

       

      Abstract: On the basis of reaction of rutin with Al3+ to form fluorescent complex, a new method for determination of rutin in tartary buckwheat by ultrasonic extraction combined with flow-injection liquid drops spectrofluorimetric was established. 10 mL methanol was added to 2.000 0 g of sample and mixed well. The mixture was ultrasonically extracted for 15 min and centrifuged at 6 000 r·min-1 for 5 min. After the supernatant was moved, the residue was extracted for twice with the same process. Then the combined supernatant were rotary evaporated to remove methanol. The sample residue was dissolved with 90% (φ) ethanol solution. After filtering, 5 μL of 0.1 mol·L-1 Al(NO3)3 solution was added and the sample solution was made up to 10.0 mL. After settling down for 60-70 min, the sample solution was flow-injected at 4-5 mL· h-1 and the fluorescence intensity of was detected at λex 239 nm and λem 507 nm. The complex ratio of Al3+:rutin is 1:2. Linear relationship was found between fluorescence intensity and mass concentration of the complex in the range of 0.10-5.00 mg·L-1, detect limit (3s) was 0.02 mg·L-1. Recovery was between 86.0% and 104%, and RSDs (n=5) were between 3.1% and 6.1%. The method was suitable for the conventional determination of rutin in tartary buckwheat.

       

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