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高效液相色谱法测定大黄酸的含量

HPLC DETERMINATION OF RHEINIC ACID

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【作者】 夏敏尹起范夏士朋上官荣昌

【Author】 XIA Min,YIN Qi-fan,XIA Shi-peng,SHANGGUAN Rong-chang(Dept.of Chemistry,Centre of Analysis and Testing,Huaiyin Teachers′ College,Huaiyin 223001,China)

【机构】 江苏省淮阴师范学院化学系分析测试中心江苏省淮阴师范学院化学系分析测试中心 淮安223300淮安223300

【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,5μm),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%.

【关键词】 高效液相色谱法大黄酸测定掌叶大黄
【Key words】 HPLCRheinic acidDeterminationChinese rhubarb
【基金】 江苏省普通高等学校高新技术产业发展项目(JH02-125)
  • 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2006年10期
  • 【分类号】R284
  • 【被引频次】5
  • 【下载频次】267
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