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[摘要]
目的 建立同时测定参丹散结胶囊丹参酮ⅡA、厚朴酚、和厚朴酚、柚皮苷、新橙皮苷、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、毛蕊异黄酮葡萄糖苷、白术内酯I 10种成分的HPLC-DAD方法。方法 采用Hypersil BDS(150 mm×4.6 mm,3.5 μm);流动相为甲醇-乙腈-0.1%磷酸水溶液,梯度洗脱,体积流量1.0 mL/min,柱温40 ℃,检测波长丹参酮ⅡA为270 nm,厚朴酚和和厚朴酚为294 nm,柚皮苷和新橙皮苷为283 nm,人参皂苷Rg1、人参皂苷Re和人参皂苷Rb1为203 nm,毛蕊异黄酮葡萄糖苷为260 nm,白术内酯I为220 nm,进样量10 μL。结果 被测定的10种成分在设定的色谱条件下均有良好的分离度,方法精密度,重复性RSD值均< 2%,被测定样品在室温条件下10 h内稳定,各成分均有较宽的线性范围和良好的线性关系,丹参酮ⅡA、厚朴酚、和厚朴酚、柚皮苷、新橙皮苷、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、毛蕊异黄酮葡萄糖苷、白术内酯I线性范围分别为112~560 μg/mL(r=0.999 6)、64~320 μg/mL(r=0.999 1)、48~240 μg/mL(r=0.999 3)、80~400 μg/mL(r=0.999 4)、80~400 μg/mL(r=0.999 5)、16~80 μg/mL(r=0.999 2)、16~80 μg/mL(r=0.999 1)、16~80 μg/mL(r=0.999 1)、40~200 μg/mL(r=0.999 2)、56~280 μg/mL(r=0.999 3),平均加样回收率在98.43%~101.52%,RSD值均< 2.0%。6批参丹散结胶囊中丹参酮ⅡA、厚朴酚、和厚朴酚、柚皮苷、新橙皮苷、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、毛蕊异黄酮葡萄糖苷、白术内酯I质量分数分别在0.829~0.840 mg/g、0.538~0.548 mg/g、0.360~0.369 mg/g、0.210~0.219 mg/g、0.111~0.118 mg/g、0.081~0.089 mg/g、0.070~0.078 mg/g、0.111~0.117 mg/g、0.072~0.080 mg/g、0.130~0.137 mg/g。结论 本方法操作简单,经方法学验证测定结果准确可靠,是可用于参丹散结胶囊的质量控制。
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[Abstract]
Objective To establish an HPLC-DAD method for the simultaneous determination of 10 components in Shendan Sanjie Capsule including tanshinone ⅡA, magnolol, honokiol, naringin, neohesperidin, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, calycosin 7-O-β-D-glucopyranoside, and atractylenolide I. Methods The chromatographic separation was performed on a Hypersil BDS column (150 mm×4.6 mm, 3.5 μm) with acetonitrile-merhanol-0.1% phosphate acid solution as mobile phase at the flow rate of 1.0 mL/min for gradient elution and the column temperature was 40 ℃. The detection wavelength was set at 270 nm for tanshinone ⅡA, 294 nm for magnolol and honokiol, 283 nm for naringin and neohesperidin, 203 nm for ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1, 260 nm for calycosin 7-O-β-D-glucopyranoside, and 220 nm for atractylenolide I. The volume of sample injection was 10 μL. Results Ten compounds were well separated under the determined chromatographic conditions. The RSD values of precision and repeatability experiment were all less than 2% and the sample solution was stable during 10 h. All the compounds had a wide linear range and good linearity: the linear range of tanshinone ⅡA, magnolol, honokiol, naringin, neohesperidin, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, calycosin 7-O-β-D-glucopyranoside, and atractylenolide I were 112—560 μg/mL (r = 0.999 6), 64—320 μg/mL (r = 0.999 1), 48—240 μg/mL (r = 0.999 3), 80—400 μg/mL(r = 0.999 4), 80—400 μg/mL (r = 0.999 5), 16—80 μg/mL (r = 0.999 2), 16—80 μg/mL (r = 0.999 1), 16—80 μg/mL (r = 0.999 1), 40—200 μg/mL (r = 0.999 2), and 56—280 μg/mL (r = 0.999 3), respectively. The average recoveries were in the range of 98.43%—101.52% and the RSD values were all less than 2.0%. The content ranges of tanshinone ⅡA, magnolol, honokiol, naringin, neohesperidin, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, calycosin 7-O-β-D-glucopyranoside, and atractylenolide I in six batches of Shendan Sanjie Capsule were 0.829—0.840 mg/g, 0.538—0.548 mg/g, 0.360—0.369 mg/g, 0.210—0.219 mg/g, 0.111—0.118 mg/g, 0.081—0.089 mg/g, 0.070—0.078 mg/g, 0.111—0.117 mg/g, 0.072—0.080 mg/g, and 0.130—0.137 mg/g, respectively. Conclusion The method is simple and convenient, the methodology validation shows that determination result of the method is accurate and reliable and it can be an effective approach for the quality control of Shendan Sanjie Capsule.
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