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目的建立高效液相色谱法测定广西不同产地金樱子药材中的芦丁、橙皮苷、槲皮素、山萘酚4个黄酮类化合物的含量。方法采用醇提法提取金樱子中的芦丁和橙皮苷,以十八烷基硅烷键合硅胶为固定相,以甲醇-0.05%磷酸水溶液作为流动相,进行梯度洗脱,柱温35℃,流速0.7ml·min~(-1),检测波长360nm。采用酸解法提取金樱子中的槲皮素和山萘酚,以十八烷基硅烷键合硅胶为固定相,以甲醇-0.1%磷酸作为流动相,进行梯度洗脱,柱温25℃,流速为0.9ml·min~(-1),检测波长360nm。结果在醇提法中,芦丁和橙皮苷两个成分的色谱峰均达到基线分离,其进样量分别在0.120~1.200μg,0.200~2.000μg范围内线性关系良好,平均加样回收率分别为100.7%和100.2%。广西不同产地金樱子中芦丁的含量为0.19~1.12mg·g-1;橙皮苷的含量为0.36~1.94mg·g-1。在酸解法中,槲皮素和山萘酚两个成分的色谱峰均达到基线分离,其进样量分别在0.070~0.700,0.036~0.360μg范围内线性关系良好,平均加样回收率分别为101.0%和98.7%。广西不同产地金樱子中槲皮素的含量为0.20~0.47mg·g-1;山萘酚的含量为0.14mg·g-1~0.39mg·g-1。结论该方法简便易行、准确、重复性好,质量控制提供参考。
OBJECTIVE To establish a HPLC method for the determination of four flavonoids, rutin, hesperidin, quercetin and kaempferol in Rosa laevigata from different areas of Guangxi. Methods Rutin and hesperidin in Rosa laevigata L. was extracted by alcohol. The elution was performed with octadecylsilane bonded silica as mobile phase and methanol-0.05% phosphoric acid as mobile phase. The column temperature was 35 ℃, flow rate 0.7ml · min ~ (-1), detection wavelength 360nm. Quercetin and kaempferol in Rosa laevigata were extracted by acid hydrolysis. Octadecylsilane bonded silica gel was used as stationary phase and methanol-0.1% phosphoric acid was used as mobile phase. The gradient elution was carried out at a column temperature of 25 ℃. The flow rate was 0.9ml · min ~ (-1) and the detection wavelength was 360nm. Results The peaks of rutin and hesperidin were all separated by baseline in alcohol extraction. The injection volumes of rutin and hesperidin were linear in the range of 0.120 ~ 1.200μg and 0.200 ~ 2.000μg, respectively. The average recovery was Respectively 100.7% and 100.2%. The content of rutin in Rosa laevigata from different areas of Guangxi was 0.19 ~ 1.12 mg · g-1, and the content of hesperidin was 0.36 ~ 1.94 mg · g-1. In the acid hydrolysis method, the chromatographic peaks of quercetin and kaempferol both reached baseline separation. The injection volumes of quercetin and kaempferol were good linearity in the range of 0.070-0.700 and 0.036-0.360 μg respectively. The average recoveries were 101.0% and 98.7%. The content of quercetin in Rosa laevigata from different areas of Guangxi was 0.20 ~ 0.47 mg · g-1, and the content of kaempferol was 0.14 mg · g-1 ~ 0.39 mg · g-1. Conclusion The method is simple, accurate, reproducible, and provides a reference for quality control.