基质固相分散-高效液相色谱法测定五味子中尼哥纳乐酸
HPLC Determination of Nigranoic Acid in Fructus Schisandra with Matrix Solid Phase Dispersion
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摘要: 提出了基质固相分散-高效液相色谱法测定五味子中的尼哥纳乐酸的方法.将样品与硅胶以质量比1比4混合研磨后装入固相萃取柱,用纯的二氯甲烷以5 mL·min-1的流量淋洗,以除去共存干扰物.用二氯甲烷-丙酮(9+1)混合液将尼哥纳乐酸从固相萃取柱上洗脱,吹氮浓缩后,以ZORBAX Stable Bound C18(4.6 mm×100 mm,1.8 μm)快速分离柱为固定相,甲醇-水(82+18)为流动相,用蒸发光散射检测器检测.峰面积与尼哥纳乐酸的质量浓度在2.0~400.0 mg·L-1范围内呈线性关系,检出限(3S/N)为20 μg·L-1.用此法分析五味子样品,所得结果的相对标准偏差(n=7)小于2.0 %,标准加入回收率在96.8%~101.5%之间.Abstract: A method of determination of nigranoic acid in fructus schisandra by HPLC with matrix solid phase dispersion was proposed.The sample was homogenized with silica gel in the ratio of 1 to 4 by mass,and packed into SPE-column.It was then eluted with pure dichloromethane at a flow rate of 5 mL·min-1 to remove co-existing interfering substances.Nigranoic acid was eluted from the column with mixed solution of dichloromethane and acetone (9+1),and then dried by blowing with N2-gas.The eluate was separated on ZORBAX Stable Bound C18 (4.6 mm×100 mm,1.8 μm) rapid column,using mixed solution of methanol and water (82+18) as mobile phase,and determined by evaporation light scattering detector.Linear relationship between the peak area and the mass concentration of nigranoic acid was obtained in the range of 2.0~400.0 mg·L-1,with detection limit (3S/N) of 20 μg·L-1.The proposed method was used in the analysis of fructus schisandras,giving RSD′s (n=7) less than 2.0%.The values of recovery found by standard addition method were in the range of 96.8%-101.5%.