高级检索

    柱前衍生-毛细管电泳法分离测定苦荞壳中的8种黄酮类化合物

    Determination of 8 Flavonoid Compounds in Tartary Buckwheat Shell by Capillary Electrophoresis after Pre-Column Derivatization

    • 摘要: 约1 g苦荞壳样品用80%(体积分数,下同)乙醇溶液5 mL于70℃搅拌提取2 h,用0.22 μm滤膜过滤,滤液于80℃水浴中灭酶30 min后,再加入2.0×10-4mol·L-1双三甲基硅烷基三氟乙酰胺(BSTFA)于80℃水浴中反应30 min,使提取液中的8种黄酮类化合物儿茶素(Cat)、芦丁(Rut)、山奈酚(Kae)、槲皮素(Mel)、金丝桃苷(Hyp)、异槲皮苷(Hir)、杨梅素(Myi)、槲皮苷(Que)衍生化。选择DB-624毛细管柱为固定相,采用含15 mmol·L-1 β-环状糊精(β-CD)的15 mmol·L-1硼酸盐溶液(pH 9.3)为运行缓冲溶液。结果显示,在最优条件下,8种黄酮类化合物衍生物可在9 min内实现快速高效的基线分离和测定。8种黄酮类化合物衍生物在一定的范围内和其对应的峰面积呈线性关系,检出限(3S/N)为0.022~0.039 mmol·L-1。以苦荞壳样品为基质进行2个浓度水平的加标回收试验,得到的回收率为99.1%~101%,测定值的相对标准偏差(n=5)为1.3%~3.2%,在苦荞壳样品中检出了5种黄酮类化合物,其质量分数为3.35~5.19 mg·kg-1

       

      Abstract: About 1 g of tartarybuck wheat shell sample was extracted with 5 mL of 80% (volume fraction, the same below) ethanol solution at 70℃ for 2 h by stirring, and the mixture was filtered by 0.22 μm filtering membrane. The filtrate was bathed at 80℃ water bath for 30 min to remove the enzyme, and then reacted with of 2.0×10-4mol·L-1 BSTFA solution in a 80℃ water bath for 30 min for derivatization of the 8 flavonoid compoundsi.e. catechins (Cat), rutin (Rut), kaempferol (Kae), quercetin (Mel), hyperin (Hyp), isoquercitrin (Hir), myricetin (Myi), quercetin (Que) in the extract. DB-624 column was selected as stationary phase, and 15 mmol·L-1 borate solution (pH 9.3) containing 15 mmol·L-1 β-CD was used as running buffer solution. It was shown by results that fast and efficient baseline separation and determination can be obtained within 9 min for the derivatives of 8 flavonoid compounds under the optimized conditions. Linear relationships between concentrations of the 8 flavonoid compound derivatives and their respective peak areas were kept within the certain ranges, with detection limits (3S/N) in the range from 0.022 mmol·L-1 to 0.039 mmol·L-1. The spiked recovery test was made at the 2 concentration levels using the tartary buckwheat shell sample as matrix, giving values of recovery in the range of 99.1%-101%, with RSDs (n=5) of determined values were ranged from 1.3% to 3.2%. The 5 flavonoid compounds were detected in the tartary buckwheat shell sample, and their values of the mass fraction found were in the range of 3.35-5.19 mg·kg-1.

       

    /

    返回文章
    返回