目的 建立药用紫草中异戊酰紫草素，乙酰紫草素，β，β-二甲基丙烯酰紫草素，异丁酰紫草素，β-乙酰氧基-异戊酰紫草素，β-羟基异戊酰紫草素，丙酰紫草素，1-甲氧基乙酰紫草素，紫草素，紫草呋喃A，紫草呋喃B，紫草呋喃D和紫草呋喃E共13个紫草素与紫草呋喃类化合物的HPLC-MS含量测定方法。方法 在负离子电离条件下，采用MRM扫描模式，以0.1%甲酸水-10 mmol·L-1甲酸铵和乙腈为流动相，以Waters Sun Fire C18column(2.1 mm×150 mm，3.5 μm)为色谱柱，在系统考察分析方法的线性、灵敏度、精密度、稳定性、重复性和加样回收率符合分析要求的基础上，对22批次市售紫草样品进行分析，准确评价紫草药材质量并分析其原因。结果 13个化合物在所选浓度范围内与峰面积呈良好线性关系，加样回收率为87.3%~107.6%，RSD值均小于9.0%。22批次市售紫草样品中的紫草素和紫草呋喃类成分存在较大差异。结论 该方法合理可行，优势明显，操作简便，可用于紫草及相关科属药用植物及其制剂的质量控制研究。
Abstract
OBJECTIVE To establish a method for simultaneous determination of 13 constituents including isovalerylshikonin, acetylshikonin, β, β-dimethylacrylshikonin, isobutyrylshikonin, β-acetoxy-isovaleryshikonin, β-hydroxyisovalerylshikonin, propionylshikonin, 1-methoxyacetylshikonin, shikonin, shikonofuran A, shikonofuran B, shikonofuran D, and shikonofuran E in Arnebia plants by HPLC-MS. METHODS The determination was performed on a Waters Sun Fire C18 column(2.1 mm×150 mm,3.5 μm)with mobile phase A consisting of water containing 0.1% formic acid and 10 mmol·L-1 ammonium formate and mobile phase B of acetonitrile under negative ionization MRM mode. The qualities of 22 batches of Arnebia plants samples obtained from medicinal materialsmarkets were investigated and evaluated after methodology validations. RESULTS There were good linear relationships between the peak areas and predetermined content ranges of these compounds. The average recoveries varied from 87.3% to 107.6%. The contents of shikonins and shikonofurans of the 22 batches of Arnebia plants samples showed significant difference. CONCLUSION The established method is feasible and simple for the quality control of Medicinal Arnebia plants and their related plants and preparations.
关键词
紫草属植物 /
液-质联用 /
紫草素 /
紫草呋喃 /
含量测定
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Key words
Arnebia plants /
HPLC-MS /
shikonin /
shikonofuran /
content determination
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中图分类号：
R917
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