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目的:建立HPLC波长切换联合梯度洗脱法测定补肾益精丸中的异去甲基蟛蜞菊内酯、蟛蜞菊内酯、金丝桃苷、紫云英苷和异鼠李素。方法:采用kromasil C18(250 mm×4.6 mm,5μm)色谱柱;流动相:乙腈(A)和0.4%磷酸溶液(B),进行梯度洗脱;流速:0.9 m L/min;柱温:30℃;进样量为20μL。异去甲基蟛蜞菊内酯和蟛蜞菊内酯的检测波长为351 nm,金丝桃苷、紫云英苷和异鼠李素的检测波长为360 nm。结果:异去甲基蟛蜞菊内酯、蟛蜞菊内酯、金丝桃苷、紫云英苷和异鼠李素分别在5.15~103.00μg/m L(r=0.999 2)、4.58~91.60μg/m L(r=0.999 8)、9.95~199.00μg/m L(r=0.999 6)、8.27~165.40μg/m L(r=0.999 9)、4.55~91.00μg/m L(r=0.999 4)范围内与峰面积具有较好的线性关系,平均加样回收率和相应的RSD(n=6)分别为97.59%(1.06%)、99.33%(1.17%)、98.18%(0.92%)、98.95%(1.11%)、97.05%(0.77%)。结论:本文建立的HPLC波长切换梯度洗脱法同时测定补肾益精丸中的5个成分:异去甲基蟛蜞菊内酯、蟛蜞菊内酯、金丝桃苷、紫云英苷和异鼠李素,方法操作简便、快速,可作为补肾益精丸全面可靠的质量控制方法。
OBJECTIVE: To establish a HPLC wavelength-switching combined gradient elution method for the determination of isodemetholide, wedelolide, hyperin, hyperin, and isorhamnetin in Bushen Yijing capsule. Methods: Kromasil C18 (250 mm × 4.6 mm, 5 μm) column was used. The mobile phase consisted of acetonitrile (A) and 0.4% phosphoric acid solution (B) ℃; injection volume of 20μL. The detection wavelength of isodemetholide and weedytholide was 351 nm, and the detection wavelength of hyperin, orientin and isorhamnetin were 360 nm. Results: The contents of isoniazid, endone, hyperin, lisin and isorhamnetin in the range of 5.15-103.00 μg / mL (r = 0.999 2), 4.58-91.60 μg / mL L (r = 0.999 8), 9.95-199.00 μg / m L (r = 0.999 6), 8.27-165.40 μg / m L (r = 0.999 9), 4.55-91.00 μg / m L The average internal standard and peak area had a good linear relationship. The average recovery rate and corresponding RSD (n = 6) were 97.59% (1.06%), 99.33% (1.17%), 98.18% (0.92%) and 98.95% (1.11%), 97.05% (0.77%). CONCLUSION: The HPLC-wavelength-switched gradient elution method established in this paper is used to determine the five components of Bushen Yijing capsule simultaneously: Isodemetholide, Wedelia lactone, Hyperin, Astilbin and Isorhamnetin , The method is simple, fast, and can be used as a comprehensive and reliable quality control method of Bushen Yijing.