期刊名称:药物分析杂志 主管单位:中国科学技术协会 主办单位:中国药学会承办:中国食品药品检定研究院 主编:金少鸿 地址:北京天坛西里2号 邮政编码:100050 电话:010-67012819,67058427 电子邮箱:ywfx@nifdc.org.cn 国际标准刊号:ISSN 0254-1793 国内统一刊号:CN 11-2224/R 邮发代号:2-237
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HPLC法测定穿龙薯蓣中薯蓣皂苷、原薯蓣皂苷和甲基原薯蓣皂苷的含量___
HPLC determination of dioscin,protodioscin and methylprotodioscin in Dioscorea nipponica Mak.
分类号:
出版年·卷·期(页码):2009,29 (5):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
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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(250 mm×4.6 mm,5 μm);流动相:乙腈(A)-水(B),梯度洗脱[0 min时A-B(5∶95),5 min时A-B(5∶95),15 min时A-B(15∶85),55 min时A-B(45∶55),65 min时A-B(100∶0),80 min时A-B(100∶0)],流速1.0 mL·min-1;检测波长208 nm;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10.08~504.0 μg·mL-1(r=09989),10.28~514.0 μg·mL-1(r=09999),10.16~508.0 μg·mL-1(r=09998);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。
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Abstract Objective:To establish a quantitative method for the determination of dioscin,protodioscin and methylprotodioscin 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,5 μm) 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 min,15%→45% A;55-65 min,45%→100% A;65-80 min,100% A.Detection wavelength was 208 nm,the column temperature was 28 ℃.Results:The method had good linear relationship within the ranges of 10.08-504.0 μg·mL-1 for dioscin(r=0.9989);10.28-514.0 μg·mL-1 for protodioscin(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 protodioscin and 99.4% for methylprotodioscin.Conclusion:The method is simple,accurate and reproducible.It provides a reliable way for evaluation the quality of Dioscorea nipponica.
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