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本文建立了虎杖中五种活性成分:虎杖苷、白藜芦醇、大黄素-8-O-β-D-葡萄糖苷、大黄素、大黄素甲醚的高效液相色谱分析方法。色谱柱为Agilent Zorbax SB C18柱(4.6×250 mm,5μm),流动相为乙腈(A)和水(B),梯度洗脱程序为:0~40 min,15.0~50.0%A;40~60 min,50.0~90.0%A。柱温为40℃,检测波长为290 nm,流速为1.0 mL/min。五种成分线性良好(R>0.999),保留时间相对标准偏差(RSD)介于0.14~1.67%,峰面积RSD介于0.96~2.96%,加标回收率介于96.8~104.7%。优化了虎杖的提取条件,最佳条件为60%乙醇超声提取30 min。对10批虎杖样品分析结果表明:虎杖苷和大黄素-8-O-β-D-葡萄苷是虎杖乙醇提取物中两种含量最高的活性成分,含量范围分别为9.80~20.42 mg/g和5.56~24.45 mg/g。白藜芦醇和大黄素的含量范围分别为1.07~5.94 mg/g和3.79~17.85 mg/g,而大黄素甲醚含量为0.57~1.69 mg/g。该高效液相色谱法重复性好、精密度高,可用于虎杖中五种活性成分的同时测定。
In this paper, a high performance liquid chromatography method for the determination of five active ingredients of Polygonum cuspidatum: polydatin, resveratrol, emodin-8-O-β-D-glucoside, emodin and physcion was established. The column was Agilent Zorbax SB C18 column (4.6 × 250 mm, 5μm) with the mobile phase of acetonitrile (A) and water (B). The gradient elution program was: 0-40 min, 15.0-50.0% A, 40-60 min, 50.0 ~ 90.0% A. The column temperature was 40 ℃, the detection wavelength was 290 nm and the flow rate was 1.0 mL / min. The five components were well linear (R> 0.999). The relative standard deviations (RSDs) of retention time ranged from 0.14 to 1.67%. The peak area RSD ranged from 0.96 to 2.96%. The spiked recoveries ranged from 96.8% to 104.7%. Optimized the extraction of Polygonum cuspidatum conditions, the best conditions for 60% ethanol ultrasonic extraction 30 min. The results of 10 batches of samples of Polygonum cuspidatum showed that polydatin and emodin-8-O-β-D-glucoside were the two most active components in the ethanol extract of Polygonum cuspidatum, and their contents ranged from 9.80 to 20.42 mg / g and 5.56 ~ 24.45 mg / g. Resveratrol and emodin contents ranged from 1.07 to 5.94 mg / g and 3.79 to 17.85 mg / g, respectively, while the content of emodin was 0.57-1.69 mg / g. The high performance liquid chromatography with good repeatability and high precision can be used for the simultaneous determination of five active ingredients in Polygonum cuspidatum.