目的 建立黑沙蒿的TLC鉴别及HPLC定量分析方法。方法 采用TLC和HPLC对采集于5个不同地区黑沙蒿进行定性和定量分析。TLC条件:对照品为斯巴醇(spathulenol),吸附剂为硅胶G,展开剂为石油醚(60~90 ℃)-丙酮(5∶)、显色剂为10%硫酸乙醇溶液;对照品为5,4′-二羟基-7-甲氧基二氢黄酮,吸附剂为硅胶G、展开剂为二氯甲烷-乙酸乙酯-甲酸(15∶1∶0.1),显色剂为紫外灯下观察。 HPLC条件:色谱柱为Topsil C18 (4.6 mm×250 mm,5 μm);流动相由水(A)和乙腈(B)组成,其梯度洗脱顺序为0~15 min,25%~38% B;15~40 min,38%~45% B,检测波长为275 nm,柱温为30 ℃。结果 对照品spathulenol和5,4′-二羟基-7-甲氧基二氢黄酮与不同样品具有Rf值相同的特征斑点,重复性好,易于鉴别;在选用的HPLC条件下,所检测化合物(1~9)表现出良好的线性关系(r>0.999 3),其平均回收率分别为97.75%、96.00%、98.20%、97.00%、95.50%、99.33%、97.50%、96.50%和97.33%,RSD均小于2.0%。化合物1、2、5、8在部分样品中没被检测到,而3、4、6、7、9均被检测到,其质量分数变化分别为(0.998±0.013)~(1.263±0.018)、(0.108±0.002)~(0.301±0.005)、(1.201±0.018)~(1.457±0.023)、(0.635±0.011)~(0.801±0.013)和(1.150±0.018)~(1.222±0.023) mg·g-1。结论 建立了黑沙蒿的TLC鉴别及HPLC定量分析方法,为综合评价该药材质量提供依据。
Abstract
OBJECTIVE To establish the TLC identification and HPLC quantitative analysis method of Artemisia ordosica. METHODS TLC and HPLC were used for qualitative and quantitative analysis of A. ordosica collected from five different regions. The TLC conditions were as follows: the reference substance was spathulenol, the adsorbent was silica gel G, the developing agent was petroleum ether (60-90 ℃)-acetone (5∶1) and the chromogenic color reagent was alcoholic solution of sulfuric acid (10%). The reference substance was 5,4′-dihydroxy-7-methoxyflavanone, the adsorbent was silica gel G, the developing agent was dichloromethane-ethyl acetate-formic acid (15∶1∶0.1) and the chromogenic reagent was ultraviolet lamp. The HPLC separation was set at performed on Topsil C18 (4.6 mm×250 mm,5 μm); the mobile phase was composed of water (A) and acetonitrile (B) and the gradient elution program was as follows: 0-15 min,25%-38% B;15-40 min,38%-45% B. The detection wavelength was 275 nm with column temperature kept at 30 ℃. RESULTS The spots of reference substances (spathulenol and 5,4′-dihydroxy-7-methoxyflavanone) and A. ordosica in TLC had good repeatability and were easy to be identified. Under the HPLC conditions adopted in this study, all calibration curves exhibited good linearity (r>0.999 3). The recoveries of the method were 97.75%, 96.00%, 98.20%, 97.00%, 95.50%, 99.33%, 97.50%, 96.50%, and 97.33%, respectively. The RSDs were less than 2.0%. Compounds 1, 2, 5 and 8 were not detected in some samples, while compounds 3, 4, 6, 7 and 9 were detected and their content changes in different samples were (0.998±0.013)-(1.263±0.018), (0.108±0.002)-(0.301±0.005), (1.201±0.018)-(1.457±0.023), (0.635±0.011)-(0.801±0.013), (1.150±0.018)-(1.222±0.023) mg·g-1, respectively. CONCLUSION The TLC identification and HPLC quantitative analysis of A. ordosica are established and can be used for the quality control of A. ordosica.
关键词
蒙药 /
黑沙蒿 /
薄层色谱法 /
高效液相色谱法 /
定量分析
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Key words
Mongolian medicine /
Artemisia ordosica /
TLC /
HPLC /
quantitative analysis
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中图分类号：
R284
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参考文献
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脚注
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基金
内蒙古自治区工程实验室开放基金项目资助(MDK2018065);蒙医药标准化国家合作科技创新项目子课题资助(MDKBZH2018017);内蒙古自治区蒙医药标准化项目资助(MB017)
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