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作 者:梁丽娟[1] 王铁杰[1,2] 冉薇[1] 李军[2] 陈晓辉[1] 钱忠直[1,3] 毕开顺[1]
机构地区:[1]沈阳药科大学药学院,沈阳110016 [2]深圳市药品检验所,深圳518029 [3]国家药典委员会,北京100061
出 处:《药物分析杂志》2009年第5期721-724,共4页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:建立同时测定穿龙薯蓣药材中薯蓣皂苷、原薯蓣皂苷和甲基原薯蓣皂苷含量的高效液相色谱方法,考察薯蓣皂苷、原薯蓣皂苷和甲基原薯蓣皂苷的含量与其产地的关系。方法:采用Shim-pack VP-ODS柱(250mm×4.6mm,5μm);流动相:乙腈(A)-水(B),梯度洗脱[0min时A-B(5∶95),5min时A-B(5∶95),15min时A-B(15∶85),55min时A-B(45∶55),65min时A-B(100∶0),80min时A-B(100∶0)],流速1.0mL·min-1;检测波长208nm;柱温28℃。结果:薯蓣皂苷、原薯蓣皂苷和甲基原薯蓣皂苷的色谱峰面积与浓度呈良好的线性关系,线性范围分别为10.08~504.0μg·mL-1(r=0.9989),10.28~514.0μg·mL-1(r=0.9999),10.16~508.0μg·mL-1(r=0.9998);平均回收率(n=9)分别为96.2%,96.3%,99.4%。结论:本测定方法简便、准确,重现性好,为穿龙薯蓣药材的质量评价提供了可靠方法。Objective: To establish a quantitative method for the determination of dioscin, protodioscin and methylp-rotodioscin in Dioscorea nipponica. Whether there is a close relation between the content and their environment in which they are living was decided. Methods : The determination was performanced on Shim - pack VP - ODS column(250 mm ×4.6 mm,5μm)with the mobile phase consisting of acetonitrile(A)and water(B) with gradient elution mode at a flow rate of 1.0 mL·min^-1. The following gradient procedure was used:0 -5 min,5% A;5 - 15 min, 5 %→15 % A; 15 - 55 rain, 15 %→45 % A ; 55 - 65 min, 45 %→100% A ;65 - 80 min, 100% A. Detection wavelength was 208 nm, the column temperature was 28 ~C. Results:The method had good linear relationship within the ranges of 10.08 -504.0 μg·mL^-1 for dioscin(r =0. 9989) ;10.28 -514.0μg·mL^-1 for protodiosein(r = 0. 9999) ;10.16 - 508.0 μg·mL^-1 for methylprotodioscin ( r = 0. 9998 ). The average recoveries ( n = 9 ) were 96.2% for dioscin ,96.3% for protodiosein and 99.4% for methylprotodioscin. Conclusion:The method is simple, accurate and reproducible. It provides a reliable way for evaluation the quality of Dioseorea nipponiea.
关 键 词:穿龙薯蓣 薯蓣皂苷 原薯蓣皂苷 甲基原薯蓣皂苷 高效液相色谱法 含量测定
分 类 号:R917[医药卫生—药物分析学]
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