首页|铁皮石斛中10种黄酮类成分UPLC-MS/MS测定与多糖组成含量分析

铁皮石斛中10种黄酮类成分UPLC-MS/MS测定与多糖组成含量分析

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目的:建立超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)同时测定铁皮石斛中10个黄酮类成分的方法,比较不同产地铁皮石斛黄酮类成分的含量差异,并结合药典指标进行系统聚类综合分析.方法:黄酮类成分测定采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×100mm,1.8 μm),以0.1％甲酸水(A)-0.1％甲酸乙腈(B)溶液为流动相,梯度洗脱,流速0.6 mL·min-1,柱温40℃,采用电喷雾离子源,负离子检测方式,得到相应的提取离子流图,以峰面积进行定量.结果:10种黄酮类成分具有良好的线性关系,r值均＞0.998 5,方法精密度、重复性和稳定性的RSD均＜3％,加样回收率在96.6％ ～ 104.7％,RSD均＜3.5％.测定结果显示不同产地铁皮石斛中黄酮类成分在组成和含量上存在较大差异;14批样品多糖、甘露糖含量均符合药典标准.结论:所建立的方法操作简便、准确、重复性好,可用于铁皮石斛药材中黄酮类成分的的定量测定,测定结果结合《中国药典》指标可为该药材质量标准的完善提供依据.
Determination of 10 Flavonoids by UPLC-MS/MS and Analysis of Polysaccharide Contents and Compositions in Dendrobii Officinalis Caulis from Different Habitats
Objective:To establish an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of ten flavonoids in Dendrobii Officinalis Caulis and compare the flavonoids and polysaccharide contents in samples from different habitats.Method:The determination was carried out by an ACQUITY UPLC BEH C1s (2.1 mm x 100 mm,1.8 μm),with 0.1％ formic acid-water (A) and 0.1％ formic acid-acetonitrile (B) as mobile phase for gradient elution.The flow rate was 0.6 mL·min-1,and the column temperature was 40 ℃.MS instrument was equipped with ESI-ion source,and the extracted ion chromatograms were obtained with negative ion detection mode,quantified by using peak area.Result:The ten flavonoid components had good linearity,r ＞ 0.998 5,and the precision,repeatability,stability and accuracy of the established method were well-validated,RSD ＜ 3％.The recovery was 96.6％-104.7％,RSD ＜ 3.5％.The results showed that there were significant differences in the composition and content of flavonoids in Dendrobii Officinalis Caulis from different habitats;the contents of polysaccharide and mannose in the 14 batches of samples were consistent with the pharmacopoeia standards.Conclusion:The established method is proved to be rapid,accurate and sensitive for the determination of flavonoids content in Dendrobii Officinalis Caulis.Moreover,the quantitative results combined with Chinese Pharmacopoeia indexes may provide basis or the improvement of quality standards of this herbal medicine.

Dendrobii Officinalis CaulisflavonoidsUPLC-MS/MSpolysaccharide

吕朝耕、杨健、康传志、李振皓、马忠华、郭兰萍、王燕萍

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中国中医科学院中药资源中心道地药材国家重点实验室培育基地,北京 100700

中国中医科学院中药资源中心无限极中药品质研究联合实验室,北京 100700

浙江寿仙谷珍稀植物药研究院,浙江武义321200

无限极(中国)有限公司,广州 510623

中国中医科学院中医临床基础医学研究所,北京 100700

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铁皮石斛 黄酮 超高效液相色谱-三重四级杆串联质谱 多糖

国家自然科学基金国家自然科学基金财政部中央本级专项发改委标准化项目浙江特色药材质量特色研究及标准制定项目浙江省重点研发项目优势特色领域重要国际标准研究项目

81325023814733072060302ZYBZH-C-HLJ-17ZH20160042017C020112016YFF02012802

2017

10.13422/j.cnki.syfjx.2017170047

中国实验方剂学杂志
中国中医科学院中药研究所　中国中西医结合学会中药专业委员会

中国实验方剂学杂志

CSTPCDCSCD北大核心
影响因子：1.62
ISSN：1005-9903
年,卷(期)：2017.23(17)
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