UPLC法同时测定何首乌中2个蒽醌糖苷

Simultaneous Determination of Two Anthraquinone Glucosides in Polygonum multiflorum Based on UPLC

目的:建立何首乌药材中大黄素-8-O-β-D-葡萄糖苷和大黄素甲醚-8-O-β-D-葡萄糖苷含量测定方法。方法:采用超高效液相色谱法,以Waters BEH C18柱(1.7μm,2.1 mm×100 mm)分离,以甲醇(A)-0.1%磷酸水溶液(B)为流动相,柱温30℃,梯度洗脱,流速为0.2 m L/min,检测波长为280 nm。结果:大黄素-8-O-β-D-葡萄糖苷进样量在0.033～0.198μg范围内与峰面积呈良好的线性关系(r=0.999 5),测得平均回收率为98.44%,RSD为1.35%;大黄素甲醚-8-O-β-D-葡萄糖苷进样量在0.024～0.144μg范围内与峰面积呈良好的线性关系(r=0.999 1),测得平均回收率为95.37%,RSD为2.41%。对不同产地16批次何首乌药材中大黄素-8-O-β-D-葡萄糖苷和大黄素甲醚-8-O-β-D-葡萄糖苷含量测定显示差异较大。结论:建立的方法简便、准确,可快速地测定出不同产地药材中2个结合性蒽醌糖苷的含量,可用于何首乌药材质量的控制。

Objective: To establish a simultaneous quantitative analytical method of emodin-8-O-β-D-glucoside and physcion-8-O-β-D-glucoside in Polygonum multiflorum Thunb. based on ultra-high performance liquid chromatography(UPLC). Methods:The UPLC method was performance on a Waters BEH C18 column(1.7 μm, 2.1 mm × 100 mm)with a binary gradient mobile phase consisting of a mixture of methanol and 0.1% aqueous phosphoric acid with column temperature at 30 ℃, and used a gradient elution method. The flow rate was set at 0.2 mL/min and the detection wavelength was set at 280 nm. Results: The calibration curve for emodin-8-O-β-D-glucoside was linear in the range of 0.033~0.198 μg(r=0.999 5).The average recovery of emodin-8-O-β-Dglucoside was 98.44%, RSD was 1.35%. The calibration curve for physcion-8-O-β-D-glucoside was linear in the range of 0.024~0.144 μg(r=0.999 1). The average recovery of physcion-8-O-β-D-glucoside was 95.37%, RSD was 2.41%. Emodin-8-O-β-Dglucoside content and physcion-8-O-β-D-glucoside content in 16 batches of Polygonum multiflorum from different regions had significant difference. Conclusion: The UPLC method is simple, sensitive and accurate with good repeatability, which is available for quality control of Polygonum multiflorum.