高效液相色谱法测定大黄酸的含量
HPLC DETERMINATION OF RHEINIC ACID
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摘要: 建立了测定大黄酸含量的高效液相色谱方法.分析柱为Waters symmetry C18色谱柱(150 mm×4.6 mm,5 μm),流动相为甲醇-水-冰乙酸(70∶30∶2,体积比),流速0.8 mL·min-1,检测波长为254 nm,回收率为99.4%-100.2%,用于原料(掌叶大黄)和产品(大黄酸)的质量控制,同一天对大黄酸标准溶液连续测定和每隔1 h进样一次测定(n=6)的相对标准偏差为0.6%-0.8%.经测定原料(掌叶大黄)中大黄酸的质量分数为0.58%,产品中大黄酸的质量分数为73.1%-90.4%.Abstract: HPLC was applied to the determination of rhein (or called rheinic acid).The Waters symmetry C18 (150 mm×4.6 mm,5 μm) was used as the stationary phase,and a mixed solution of methanol,water and acetic acid in the ratio of 70 to 30 to 2 (by volume) was used as the mobile phase.UV-detection at the wavelength of 254 nm was used.The flow-rate of mobile phase was 0.8 mL·min-1.Precision tests of within-day and between-days repeatability,and of reproducibility in the same laboratory were performed,and RSD′s (n=6) of repeatability obtained were in the range of 0.6%-0.8% and RSD (n=6) of reproducibility was 0.7%.Recovery were tested at 3 different concentration levels giving values in the range of 99.4%-100.2%.In the determination of rheinic acid in its raw material (palmate leaf chinese rhubarb) and products,0.58% of rheinic acid was found in the raw material,and contents of rheinic acid in the products were in the range of 73.1%-90.4%.