大豆异黄酮的测定方法研究  

A study on methods for determination of soy isoflavones in soy and soy-based products

作　　者：常凤启[1] 秦振顺[1] 韩会新[1] 杨娜敬[1] 刘玉欣[1] 

机构地区：[1]河北省疾病预防控制中心,河北保定071000

出　　处：《中国卫生检验杂志》2006年第2期131-134,139,共5页Chinese Journal of Health Laboratory Technology

基　　金：国家科技计划攻关课题资助项目(2001BA804A21)

摘　　要：目的：检测大豆及其制品中黄豆甙、大黄豆甙、染料木甙、黄豆甙元、大黄豆索和金雀异黄素，建立大豆及其制品中6种大豆异黄酮的高效液相色谱-二极管阵列检测器（HPLC-PDA）检测方法。方法：保健食品、豆腐等样品中的大豆异黄酮直接用甲醇水（80＋20，v／v）超声提取30min，定容过0．45μm滤膜后测定；豆粉和豆奶粉等样品中的大豆异黄酮及其酯类用甲醇水（80＋20，v／v）超声提取，提取液经碱性皂化，将某些酯类转化成对应的大豆异黄酮，经盐酸中和，甲醇水（80＋20，v／v）定容，过滤膜后测定；酱油和豆豉等样品超声提取30min，提取液经OASIS HLB柱去杂质，过0．45μm滤膜，进行液相色谱分析。样品中的6种大豆异黄酮用甲醇和醋酸铵（0．025mol／L，pH4．1）作流动相，流速2．0ml／min进行梯度洗脱，经250×4．6mm粒径10μm C18柱分离，二极管阵列检测器（210～400nm）测定。30min内6种大豆异黄酮可得到良好分离。结果：测定6种大豆异黄酮的平均加标回收率在86．7％-116％，加标回收相对标准偏差均小于8％，最底检出限量小于0．04μg。结论：本方法适用于大豆及其制品中大豆异黄酮的测定。Objectlve：To develop a method based on HPLC - PDA for determination of 6 soy isoflavones in soy and soy - based products. Methods： After being sonicated for 30 min and filtered through 0.45 μm filter, the analytes extracted from health foods and Tofu were analyzed by a gradient elution HPLC - PDA system and those from bean powder were hydrolyzed with sodium hydroxide before HPLC analysis. The analytes from soy sauce and fermented soya beans were isolated and concentrated by solid - phase extraction before HPLC analysis. The samples were separated on a C18 reversed -phase column using methanol： 0. 025 mol/L ammonium acetate pH 4. 1 as the mobile phase at a velocity of 2. 0 mE/rain and detected by photodiode - array detector at 210 - 400 nm. Good separation of daidzin, glycitin, genistin, daidzein, glycitein and genistein was achieved in about 30 min. Results： The average recovery of 6 isoflavones was within 86.7% - 116%, and the relative variation coefficient was below 8% for all. The minimal detecting amount of the 6 soy isoflavones was below 0. 04 μg. Conclusion： This method is suitable for the determination of soy isoflavones in soy and soy - based products.

关 键 词：大豆制品 异黄酮类 色谱法 高效液相 

分 类 号：O657.72[理学—分析化学]