[关键词]
[摘要]
目的 建立HPCE-DAD法测定鬼针草中10种酚类化合物(木犀草苷、芦丁、槲皮素-3-O-葡萄糖苷、槲皮苷、水杨酸、木犀草素、山柰酚、槲皮素、没食子酸和原儿茶酸)的方法,比较6种不同体积分数的乙醇对上述化合物提取效率的影响。方法 实验考察了缓冲液pH、浓度、分离电压、毛细管冷却液温度等因素对分离的影响。在214 nm检测波长下,60 cm长毛细管中,25 mmol/L硼砂(pH 9.5),分离电压25 kV,毛细管冷却液温度25 ℃时上述各化合物在16 min内能得到完全分离。结果 木犀草苷、芦丁、槲皮素-3-O-葡萄糖苷、槲皮苷、水杨酸、木犀草素、山柰酚、槲皮素、没食子酸和原儿茶酸分别在5.0~120、5.0~120、5.0~120、5.0~120、1.0~120、2.5~120、5.0~120、2.5~120、2.5~120、2.5~120 mg/L与其峰面积呈线性关系,其检出限分别为2.5、2.5、2.5、2.5、0.5、1.0、2.5、1.0、1.0、1.0 mg/L,精密度RSD≤5.17%(n=6),测定样品的加样回收率在94.4%~105.8%,RSD在0.32%~4.33%。结论 鬼针草中木犀草苷、芦丁、槲皮素-3-O-葡萄糖苷、槲皮苷、水杨酸、木犀草素、山柰酚、槲皮素、没食子酸和原儿茶酸的量分别为95.04~105.84、78.03~110.45、96.45~177.96、178.78~300.00、62.06~66.54、71.08~72.85、77.39~95.30、68.27~77.43、68.47~88.47、107.24~142.43 μg/g。
[Key word]
[Abstract]
Objective To develop a novel method using high-performance capillary electrophoresis coupled with DAD (HPCE-DAD) for the simultaneous determination of 10 phenolic compounds (luteolin-7-O-glucoside, rutin, quercetin-3-glucoside, quercetin-3- rhamnoside, salicylic acid, luteolin, kaemferol, quercetin, gallic acid, and protocatechuic acid) in Bidens bipinnata. The extraction efficiency of above mentioned compounds was compared using six different ethanol/water solutions. Methods The effects of pH value and concentration of buffer, applied voltage, and temperature on the separation were researched. The 10 compounds were baseline separated within 16 min in a 60 cm length capillary at a separation voltage of 25 kV with a running buffer consisting of 25 mmol/L borate (pH 9.5) at wavelength of 214 nm. Results Excellent linearities of luteolin-7-O-glucoside, rutin, quercetin-3-glucoside, quercetin-3-rhamnoside, salicylic acid, luteolin, kaemferol, quercetin, gallic acid, and protocatechuic acid were observed at 5.0-120, 5.0-120, 5.0-120, 5.0-120, 1.0-120, 2.5-120, 5.0-120, 2.5-120, 2.5-120, and 2.5-120 mg/L, respectively. The detection limits were at 2.5, 2.5, 2.5, 2.5, 0.5, 1.0, 2.5, 1.0, 1.0, and 1.0 mg/L, respectively. The relative standard deviations (RSD) of precision were below 5.17% (n = 6). The mean recoveries for 10 phenolic compounds in B. bipinnata ranged from 94.4% to 105.8%, with RSD values of 0.32%-4.33%. Conclusion The contents of luteolin-7-O-glucoside, rutin, quercetin-3- glucoside, quercetin-3-rhamnoside, salicylic acid, luteolin, kaemferol, quercetin, gallic acid, and protocatechuic acid in B. bipinnata are 95.04-105.84, 78.03-110.45, 96.45-177.96, 178.78-300.00, 62.06-66.54, 71.08-72.85, 77.39-95.30, 68.27-77.43, 68.47-88.47, and 107.24-142.43 μg/g, respectively.
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[基金项目]
安徽高校省级科学研究项目(KJ2013Z139);安徽医科大学校科学研究项目(2012xkj018)