黑米中矢车菊色素的提取工艺优化及测定Optimization and Determination of Extraction Process of Cyanidin Pigment from Black Rice
廖若宇,刘新保,张春娥,孙悦,谭梦瑶
摘要(Abstract):
建立了一种黑米中矢车菊色素的提取与测定方法。利用单因素试验对提取过程中的各项因素进行优化,然后通过响应面试验确定料液比、振荡提取时间及水浴振荡温度3个因素的最优组合条件。由试验可得液相色谱测定方法为:色谱柱:Inertsil ODS-SP C18(250 mm×4.6 mm, 5μm),检测波长:520 nm,柱温:30℃,流动相:0.5%的甲酸水溶液和0.5%的甲酸甲醇溶液(45∶55,V/V)等度洗脱,流速:1.0 mL/min,进样体积:10μL。最优提取条件为:95%乙醇和盐酸混合液提取,当料液比为0.5∶15、提取次数为2次、提取温度为70℃、超声时间为5 min、恒温振荡25 min时,离心合并提取液,得到黑米中矢车菊色素含量为3.972 mg/g。文章还首次引入了Sep-Pak Vac 3cc NH2 Cartridges固相萃取柱,试验表明经过净化后的样品,其色谱图基线更加平稳,杂质干扰小,色谱峰分离度更好,能够有效减少色谱柱的污染,但存在部分色素损失,损失量在0.5 mg/g范围内。文章建立的方法绿色高效、操作简单,能够有效提取黑米中的矢车菊色素。
关键词(KeyWords): 黑米;矢车菊色素;提取;液相色谱仪;固相萃取柱
基金项目(Foundation): 宁夏回族自治区重点研发项目(2018BEG03070)
作者(Author): 廖若宇,刘新保,张春娥,孙悦,谭梦瑶
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