[关键词]
[摘要]
目的 建立HPLC法同时测定大黄中5种游离型蒽醌(芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚)、4种结合型蒽醌(芦荟大黄素-8-O-葡萄糖苷、大黄素-1-O-葡萄糖苷、大黄酚-1-O-葡萄糖苷和大黄素-8-O-葡萄糖苷)及没食子酸、儿茶素共计11种成分的定量方法。方法 采用Symmetry C18色谱柱,流动相为甲醇-0.1%磷酸水梯度洗脱,体积流量1.0 mL/min,柱温30℃,检测波长254 nm。结果 没食子酸、儿茶素、芦荟大黄素-8-O-葡萄糖苷、大黄素-1-O-葡萄糖苷、大黄酚-1-O-葡萄糖苷、大黄素-8-O-葡萄糖苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在0.062 4~1.560 0、0.180 0~4.500 0、0.041 2~1.030 0、0.030 6~0.765 0、0.051 0~1.275 0、0.028 8~0.720 0、0.019 8~0.495 0、0.050 5~1.262 5、0.063 7~1.592 5、0.098 0~2.450 0和0.163 0~4.075 0 μg进样量与峰面积积分值线性关系良好(r≥0.999 5),平均加样回收率为95.37%~98.93%,RSD<2.36%。结论 该法简便、准确、专属性强,可用于大黄中11种成分的测定。
[Key word]
[Abstract]
Objective To establish an HPLC method for the simultaneous determination of five free anthraquinones (aloe-emodin, rhein, emodin, chrysophanol, and physcion), four bound anthraquinones (aloe-emodin-8-O-glucopyranoside, emodin-1-glucoside, chrysophanol-1-glucoside, and emodin-8-glucoside), gallic acid, and catechin in Rhei Radix et Rhizome. Methods The analysis was achieved with a Symmetry C18 column by gradient elution of methanol-0.1% phosphoric acid in water at 30℃. The flow rate was 1 mL/min, and the detection wavelength was set at 254 nm. Results The calibration curves of all eleven constituents showed good linearity (r ≥ 0.999 5) in a relatively wide concentration range. The linear ranges of gallic acid, catechin, aloe-emodin-8-O-glucopyranoside, emodin-1-O-glucoside, chrysophanol-1-O-glucoside, emodin-8-O-glucoside, aloe-emodin, rhein, emodin, chrysophanol, and physcion were 0.062 4-1.560 0, 0.180 0-4.500 0, 0.041 2-1.030 0, 0.030 6-0.765 0, 0.0510 0-1.275 0, 0.028 8-0.720 0, 0.019 8-0.495 0, 0.050 5-1.262 5, 0.063 7-1.592 5, 0.098 0-2.450 0, and 0.163 0-4.075 0 μg (r ≥ 0.999 5), respectively. The mean recovery of these eleven components was 95.37%-98.93%, RSD < 2.36%. Conclusion This method is simple, accurate, and specific, and can be used for the determination of eleven constituents in Rhei Radix et Rhizome.
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[基金项目]
江苏省第4期“333工程”资助科研项目(BRA2013090);江苏省中医药局科技项目(LZ13168);江苏省南通市应用研究计划项目(BK2013013)