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Alhima ODS(250mm×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1.0mL·min^-1,检测波长为254nm(测定五味子醇甲)、284nm(测定仙茅苷、丹皮酚、哈巴俄苷)、330nm(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 simultaneous determination of six active ingredients (2,3,5,4' - tetrahydroxystilbene -2-O-β-D- glucoside, acteoside, curculigoside, paeonol, harpagoside, schisandrin). Methods:The determination was carried out with Alltima ODS column (250 mm× 4.6 mm, 5 μm) ; The mobile phase consisted of acetonitrile (A) -0.05 % phosphoric acid solution (B) with gradient elution at a flow rate of 1.0 mL · min^-1; The detection wavelengths were 254 nm for schisandrin, 284 nm for curculigoside, paeonol and harpagoside, 330 nm for 2,3,5,4' - tetrahydroxystilbene -2-O-β-D- glucoside and acteoside. Results: The calibration curves were linear in the ranges of 0. 0404 - 1. 616 μg for 2,3,5,4' - tetrahydroxystilbene -2-O-β-D- glucoside( r = 0. 9999 ), 0. 0194 - 0. 774 μg for acteoside ( r = 0. 9998 ) , 0. 0202 - 0. 810 μg for curculigoside (r =0. 9997), 0. 0201 -0. 804 μg for paeonol (r =0. 9999), 0. 0206 -0. 826 μg for harpagoside(r =0. 9998), 0. 0398 - 1. 592 μg for schisandrin (r = 0. 9999) ; The average recoveries (n = 6) were 97.8%, 98.2%, 97.9%, 98.3% , 101.2% , and 97.5% ; RSDs were 1.2% , 1.1% , 0. 95% , 1.1% , 0. 97% , and 1.1% , respectively. Conclusion : The method is simple and repeatable, which can be applied to the quality control of Gengnian' an tablets.