Box-Behnken设计-响应面法优化三棱总黄酮的分离纯化工艺研究
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摘要
目的:优化三棱总黄酮的纯化工艺。方法:采用大孔吸附树脂分离纯化法,以上样液pH、洗脱液流速、洗脱液浓度为考察因素,总黄酮纯化率为评价指标,在单因素试验的基础上采用Box-Behnken设计-响应面法优化三棱总黄酮的纯化工艺,并进行验证试验。结果:最优纯化工艺为上样液pH为4.8、洗脱液流速为2.0 BV/h、洗脱液浓度为72%;验证试验中3批样品纯化后的总黄酮纯化率为72.34%(RSD=1.77%,n=3),与预测值(73.99%)的相对误差为2.13%。结论:优选的纯化工艺方法稳定、可行,可用于三棱总黄酮的纯化。
OBJECTIVE: To optimize the purification technology of total flavonoids from Sparganium stoloniferum.METHODS:Separation and purification by macroporus adsorption resin,using sample solution pH,flow rate and concentration of eluent,the purification rate of total flavonoids as evalution indexes,the purification technology of total flavonoids from S.stoloniferum were optimized by Box-Behnken design-response surface methodology based on single factor test. Validation test was conducted. RESULTS: The optimal purification technology was sample solution pH 4.8, flow rate of eluent 2.0 BV/h,concentration of eluent 72%. The purification rate of total flavonoids in 3 batches of samples was 72.34%(RSD=1.77%,n=3)in validation test,relative errors of which to predicted value(73.99%) was 2.13%. CONCLUSIONS:The optimal purification technology is stable and feasible,and can be used for the purification of total flavonoids from S. stoloniferum.
OBJECTIVE: To optimize the purification technology of total flavonoids from Sparganium stoloniferum.METHODS:Separation and purification by macroporus adsorption resin,using sample solution pH,flow rate and concentration of eluent,the purification rate of total flavonoids as evalution indexes,the purification technology of total flavonoids from S.stoloniferum were optimized by Box-Behnken design-response surface methodology based on single factor test. Validation test was conducted. RESULTS: The optimal purification technology was sample solution pH 4.8, flow rate of eluent 2.0 BV/h,concentration of eluent 72%. The purification rate of total flavonoids in 3 batches of samples was 72.34%(RSD=1.77%,n=3)in validation test,relative errors of which to predicted value(73.99%) was 2.13%. CONCLUSIONS:The optimal purification technology is stable and feasible,and can be used for the purification of total flavonoids from S. stoloniferum.
引文
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[13]李傲,徐晓玉,董伟,等.三棱丸抑制大鼠异位子宫内膜芳香化酶及环氧合酶-2表达的研究[J].中国中药杂志,2008,33(11):1297-1301.
[14]沈东成,徐秋霞,余舒鹏,等.生三棱-生莪术组分配伍对卵巢囊肿大鼠雌激素受体的作用研究[J].江西中医药大学学报,2017,29(2):68-69,103.
[15]王恒,李伟东.三棱薄层色谱鉴别及总黄酮的含量测定[J].成都中医药大学学报,2016,39(1):10-14.
[2]毛淑杰,王素芬,李文,等.三棱不同炮制品抗血小板聚集及对凝血时间的影响[J].中国中药杂志,1998,23(10):29-30.
[3]和岚,张秀梅,毛腾敏.三棱、丹参对血液流变学影响的比较研究[J].山东中医药大学学报,2007,30(5):434-435.
[4]邱才炜,徐晓玉,祝慧凤.三棱丸抗炎镇痛作用研究[J].中药药理与临床,2008,24(5):7-10.
[5]孟冰,闵冬雨,谷淑玲.5种中药对脑缺血缺氧损伤的保护作用[J].徐州医学院学报,2009,29(9):615-617.
[6]孙杰,王芍,郭斌,等.三棱黄酮体外诱导A549及MCF-7细胞S/G_2周期停滞的研究[J].天然产物研究与开发,2011,23(2):224-227,282.
[7]孙杰,王芍,郭斌,等.三棱黄酮抗HeLa宫颈癌:降低分裂期细胞比率诱导细胞凋亡[J].食品科学,2011,32(1):210-214.
[8]冯娅茹,张文婷,李二文,等.三棱化学成分及药理作用研究进展[J].中草药,2017,48(22):4804-4818.
[9]胡旭光,邓小慧,李淑贤,等.不同三棱提取物药理活性的比较研究[J].陕西中医,2009,30(8):1091-1093.
[10]李可意,刘红梅.高效液相色谱法测定三棱超临界萃取物中芦丁的含量[J].时珍国医国药,2008,19(3):684-685.
[11]LEE SY,CHOI SU,LEE JH,et al.A new phenypropaneglycoside from the rhizome of Sparganium stoloniferum[J].Arch Pharm Res,2010,33(4):515-521.
[12]余成浩,彭腾,杜洁,等.“三棱-莪术”组分配伍对大鼠子宫肌瘤的影响[J].中药药理与临床,2014,30(3):104-107.
[13]李傲,徐晓玉,董伟,等.三棱丸抑制大鼠异位子宫内膜芳香化酶及环氧合酶-2表达的研究[J].中国中药杂志,2008,33(11):1297-1301.
[14]沈东成,徐秋霞,余舒鹏,等.生三棱-生莪术组分配伍对卵巢囊肿大鼠雌激素受体的作用研究[J].江西中医药大学学报,2017,29(2):68-69,103.
[15]王恒,李伟东.三棱薄层色谱鉴别及总黄酮的含量测定[J].成都中医药大学学报,2016,39(1):10-14.