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目的:建立同时分析测定更年安片中6个活性成分(2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、毛蕊花糖苷、仙茅苷、丹皮酚、哈巴俄苷、五味子醇甲)的方法。方法:采用HPLC-DAD法,色谱柱为奥泰Alltima ODS(250 mm×4.6mm,5μm),以乙腈为流动相A,0.05%磷酸溶液为流动相B,梯度洗脱,流速1.0 mL.min-1,检测波长为254 nm(测定五味子醇甲)、284 nm(测定仙茅苷、丹皮酚、哈巴俄苷)、330 nm(测定2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、毛蕊花糖苷)。结果:2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、毛蕊花糖苷、仙茅苷、丹皮酚、哈巴俄苷、五味子醇甲线性范围分别为0.0404～1.616μg(r=0.9999),0.0194～0.774μg(r=0.9998),0.0202～0.810μg(r=0.9997),0.0201～0.804μg(r=0.9999),0.0206～0.826μg(r=0.9998),0.0398～1.592μg(r=0.9999)。平均加样回收率(n=6)分别为97.8%,98.2%,97.9%,98.3%,101.2%,97.5%;RSD分别为1.2%,1.1%,0.95%,1.1%,0.97%,1.1%。结论:该方法操作简单,重复性好,为评价和监控更年安片的质量提供可靠的方法。
OBJECTIVE: To establish a method for the simultaneous determination of six active ingredients (2,3,5,4’-tetrahydroxystilbene-2-O-β-D-glucoside, verbascoside, curculin, Phenol, Harpagoside, Schizandrol A). Methods: The HPLC-DAD method was used. The column was Altai Alltima ODS (250 mm × 4.6 mm, 5 μm) with acetonitrile as mobile phase A and 0.05% phosphoric acid as mobile phase B with gradient elution at a flow rate of 1.0 mL · min -1, the detection wavelength was 254 nm (determination of Schisandrin A), 284 nm (curculin, paeonol, harpagoside), 330 nm (measured 2,3,5,4’-tetrahydroxystilbene -2-O-β-D-glucoside, verbascoside). Results: The linear ranges of 2,3,5,4’-tetrahydroxystilbene-2-O-β-D-glucoside, verbascoside, curculigoside, paeonol, harpagoside and schisandrin were (R = 0.9999), 0.0204 ~ 1.616μg (r = 0.9999), 0.0194 ~ 0.774μg (r = 0.9998), 0.0202 ~ 0.810μg 0.0398 ~ 1.592μg (r = 0.9999). The average recovery was 97.8%, 98.2%, 97.9%, 98.3%, 101.2% and 97.5%, respectively. The RSDs were 1.2%, 1.1%, 0.95%, 1.1%, 0.97% and 1.1% . Conclusion: The method is simple, reproducible and provides a reliable method for evaluating and monitoring the quality of GMP.