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反相高效液相制备色谱法分离淡豆豉中的大豆苷、黄豆苷、染料木苷 被引量:8

Separation of soybean isoflavone glucosides from Semen Sojae Praeparatum by preparative reversed-phase high performance liquid chromatography
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摘要 目的:建立一种快速、高效地从淡豆豉的乙醇提取物中分离3种大豆异黄酮苷的方法。方法:采用索氏提取除去脂溶性成分,再经1300型大孔吸附树脂初步分离纯化,分别用水、10%、20%、30%、40%、50%、70%、95%乙醇梯度洗脱,其中对40%乙醇洗脱流分采用反相高效液相色谱法制备,色谱条件:YWG C18柱(10.0 mm×200 mm,10μm),进样量750μl,乙腈-水-冰醋酸(25:75:1,V/V/V)为流动相,流速3.0 m l/m in,检测波长260 nm。结果:快速分离得到大豆苷、黄豆苷和染料木苷,经外标法检测,所得化合物纯度均达到99%以上。结论:该方法操作简便,可重复进样,适用于高纯度大豆异黄酮苷的制备。 Objective:To search for a rapid and efficient method for the isolation of 3 kinds of isoflavone glucosides from the ethanol extract of Semen Sojae Praeparatum. Methods: The crude isoflavones were extracted by 75 % aqueous ethanol after removing the oil by Soxhlet extraction. Then 1300 macroporous resin, water and different concentrations of aqueous ethanol (10%, 20%, 30%, 40%, 50%, 70%, and 95%) were used to separate and elute the crude isoflavones. The fraction eluted by 40% aqueous ethanol was subjected to preparative HPLC analysis. The chromatographic conditions: A YWG C18 (10.0 mm×200 mm, i. d. 10 μm) column was used; the mobile phase consisted of acetonitrile water-acetic acid at volume ratio of 25 : 75 : 1 (V/V/V) and a flow rate of 3.0 ml/min; the injection volume was 750 μl; and the detection wave length was set at 260 nm. Results: Daidzin, glycitin and genistin were rapidly separated with the purities over 99% as determined by external standard HPLC. Conclusion: This technique is simple and suitable for the isolation of daidzin, glycitin and genistin from Semen Sojae Praeparatum.
出处 《第二军医大学学报》 CAS CSCD 北大核心 2006年第3期325-326,共2页 Academic Journal of Second Military Medical University
基金 上海市科技发展基金(02DZ19111)~~
关键词 色谱法 高效液相 淡豆豉 大豆苷 黄豆苷 染料木苷 chromatography,high performance liquid Semen Sojae Praeparatum daidzin glycitin genistin
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