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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,3.5μm)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。
OBJECTIVE To establish a method for the determination of isovaleramine, acetylshikonin, β, β-dimethylacrylshikonin, isobutyryl shikonin, β-acetoxy-isovalerate Β-hydroxyisovaleryl shikonin, propionate shikonin, 1-methoxyacetyl shikonin, shikonin, comfrey A, comfrey B, comfrey D and comfrey E Determination of 13 shikonin and comfrey furan compounds by HPLC-MS method. Methods Under the negative ionization conditions, the column was equipped with a Waters Sun Fire C18column (2.1 mm × 150 mm, 3.5 μm) column using MRM scanning mode with 0.1% formic acid-10 mmol·L-1 ammonium formate and acetonitrile as mobile phase On the basis of that the linearity, sensitivity, precision, stability, repeatability and recovery rate of systematic investigation and analysis meet the analytical requirements, 22 batches of comfrey samples were analyzed to evaluate the quality of comfrey Analysis of the reasons. Results Thirteen compounds showed a good linear relationship with the peak area in the range of concentration. The recoveries were 87.3% -107.6% with RSD less than 9.0%. 22 batches of comfrey and comfrey furan components in the sample of comfrey there is a big difference. Conclusion The method is reasonable and feasible, with obvious advantages and simple operation, which can be used for the quality control of medicinal plants and their preparations of Lithospermum and related families.