摘要
目的建立唐古特瑞香药材中4种主要成分的HPLC测定方法,并进行聚类分析。方法:采用高效液相色谱法。色谱柱为Teckmeck C_(18)(5μm,4.6 mm×250 mm);流动相A:乙腈,流动相B:0.4%磷酸,梯度洗脱(0~40 min,A:15%→30%;40~45 min,A:30%→15%;45~50 min,A:15%);检测波长为266 nm,流速1.0 mL·min~(-1),柱温为35℃,进样量为20μL。结果祖师麻甲素、芫花素、紫丁香苷、7-羟基香豆素检测质量浓度线性范围分别为0.4112~205.6μg·m L~(-1)(r=0.9999)、0.4348~217.40μg·m L~(-1)(r=0.9999)、0.4104~205.2μg·m L~(-1)(r=0.9999)、0.4276~213.80μg·m L~(-1)(r=0.9999);精密度、稳定性、重复性试验的RSD均<2.0%;加样回收率为97.4%~101.3%(RSD=0.80%~1.3%,n=6)。10批次样品可聚为2类,产地为青海海北州门源县与青海湟中县样品所含成分含量相近。结论建立的含量测定方法操作简单,精密度、稳定性、重复性好,可用于同时测定唐古特瑞香药材中祖师麻甲素、芫花素、紫丁香苷、7-羟基香豆素的含量;不同产地的唐古特瑞香药材成分含量差异较大。
Objective To establish a method for the simultaneous determination of 4 components in Daphne tangutica Maxim and to conduct cluster analysis. Methods HPLC method was adopted. The determination was performed on Teckmeck C_(18)(5 μm, 4.6 mm×250 mm) column with mobile phase consisting of acetonitrile-0.4% phosphate acid solution(gradient elution) at the flow rate of 1.0 mL·min~(-1). The detection wavelength was 266 nm and the column temperature was 35℃. The injection volumn was 20 μL. Results The linear ranges of daphnetin, genkwanin, syringin, and 7-hydroxycumarin were 0.4112-205.6 μg·m L~(-1)(r =0.9999), 0.4348-217.40 μg·mL~(-1)(r = 0.9999), 0.4104-205.2 μg·mL~(-1)(r = 0.9999), and 0.4276-213.80 μg·mL~(-1)(r = 0.9999), respectively. The RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The recoveries were 97.4%-101.3%(RSD = 0.80%-1.3%, n = 6). The 10 batches of medicinal materials could be divided into 2 categories. Conclusion The method is simple, precise, stable and reproducible, and it can be used for the simultaneous determination of 4 components in Daphne tangutica Maxim. The quality of Daphne tangutica Maxim from different regions is quite different.
引文
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