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作 者:夏敏[1] 尹起范[1] 夏士朋[1] 上官荣昌[1]
机构地区:[1]江苏省淮阴师范学院化学系分析测试中心,淮安223300
出 处:《理化检验(化学分册)》2006年第10期832-833,835,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:江苏省普通高等学校高新技术产业发展项目(JH02-125)
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Waterssy Tnmetry C18色谱柱(150min×4·6mm,5μm),流动相为甲醇-水-冰乙酸(70:30:2,体积比),流速0.8mL·min^-1。检测波长为254nm,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1h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%。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%.
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