正交实验优化柚皮中柚皮苷的超声辅助双水相提取工艺

Ultrasonic-assisted Aqueous Two-phase Extraction of Naringin from Pomelo Peel by Orthogonal Experimental Design

采用超声辅助正丙醇/(NH_4)_2SO_4双水相萃取技术对菊花芯柚果皮中柚皮苷的提取分离工艺进行系统研究。采用单因素均分法系统考察了(NH_4)_2SO_4质量分数、正丙醇质量分数、柚皮干粉加入量、pH、温度和时间6种关键因素对柚皮苷得率的影响,通过正交实验设计确定了双水相萃取技术最优工艺条件,并进行了放大实验研究和对比实验。结果表明,柚皮苷主要富集于上相,在优水平下,构建10.0 g双水相体系,正丙醇质量分数为21%(w/w),(NH_4)_2SO_4质量分数为18%(w/w),柚皮干粉加入量为0.15 g,调节pH至4.5,40℃条件下,超声提取30 min,柚皮苷得率为4.27%,RSD为1.23%,100倍放大后柚皮苷得率达到4.25%。对比热回流提取,正丙醇/(NH_4)_2SO_4双水相提取具有提取时间短、温度低、能耗小、效果好等优点,优势明显,可以实现柚皮中柚皮苷的有效分离,为工业制备柚皮苷提供了一种新途径。

An ultrasonic- assisted technology combined with 1- propanol and （NH_4）_2SO_4 aqueous two-phase system was developed for the extraction and purification of naringin from the peel of chrysanthemum core pomelo.According to the literature and preliminary studies, the influence factors of 1 - propanol mass fraction, （NH_4）_2SO_4 mass fraction, sample loading, pH, ultrasonication temperature and time were investigated by single factor designs.Subsequently, the impact of various factors to optimize the process were analyzed by orthogonal experiment.Furthermore,scale-up experiment and comparison test were also been assessed.Results showed that ：Naringin was mainly extracted into the top phase, and the optimal experimental conditions of 10.0 g 1- propanol/salt aqueous two-phase system, 1- propanol mass fraction of 21% （w/w）, （NH_4）_2SO_4 mass fraction of 18% （w/w） ,sample loading at 0.15 g, pH at 4.5, temperature at 40 ℃, time at 30 rain. Under the optimal condition, the maximum yield of naringin was 4.27%, RSD was 1.23% .The 100 times scale-up results showed that the yield was 4.25% .The comparison results indicated that ultrasonic- assisted aqueous two- phase extraction was more efficient than heat reflux extraction,which had the shorter extraction time, the lower extraction temperature and the higher extraction efficiency. The ultrasonic-assisted aqueous two- phase method was suitable for the separation and enrichment of naringin from peel of chrysanthemum core pomelo.And it could provide a new way for the preparation of naringin in industrial field.