超高压辅助超声波法提取紫玉米籽粒花色苷的工艺研究

Study on Extraction of Anthocyanins from Purple Corn Seeds by Ultra-high-Pressure Assisted Ultrasonic Method

超声波和超高压提取通常单独应用于植物花色苷的提取过程,现将两种技术结合来提取紫玉米籽粒花色苷,以提高紫玉花色苷的提取率及提取效率。以紫玉米籽粒为原料,料液比为1∶16g·mL^(-1)的无水乙醇:0.2mol·L^(-1)柠檬酸溶液(7∶3)为提取溶剂,以超高压压力、超高压时间、超声波时间为考察因素进行单因素试验,并通过响应面优化实验来获得最佳的提取工艺。结果表明:花色苷最佳提取工艺为:超高压压力为270MPa、超高压时间为1.9min、超声时间为8.5min,在此工艺条件下,花色苷提取的最大值为49.68mg·100g^(-1),达到理论预测值的99.31%。此方法较单一超声波提取,其提取率增加17.80%,提取时间缩短30.58%;结合提取所得花色苷提取液1,1-二苯基-2-三硝基苯肼(DPPH)自由基清除率为57.62%,2,2-联氮双(3-乙基苯并噻唑啉-6-磺酸)二铵盐(ABTS)自由基清除率为44.83%,单一超声波提取所得花色苷提取液DPPH自由基清除率为54.74%,ABTS自由基清除率为42.48%,可见,超高压结合超声波提取有效提高了花色苷提取率,及对DPPH自由基和ABTS自由基的清除能力。对结合提取和单一超声波提取两种提取方式所得到的紫玉米籽粒花色苷组成进行液相色谱-质谱联用(HPLC-MS)技术定性分析和定量测定,两种提取方式共分离出12种花色苷,其中,单一超声波提取不含矢车菊素-3-O-二丙二酰基葡萄糖苷,结合提取不含锦葵素-3-O-葡萄糖苷;两种提取方式共同含有的10种花色苷中天竺葵素-3-O-丙二酰基葡萄糖苷含量最高,芍药素-3-O-葡萄糖苷含量最低。

Ultrasonic and ultra-high pressure extraction are usually used in the process of plant anthocyanin extraction alone.Now,the two technologies are combined to extract anthocyanins from purple corn seeds,so as to improve the extraction rate and efficiency of anthocyanins from purple jade.Purple corn seeds were used as raw materials,the ratio of solid to liquid was 1∶16g·mL^(-1) of absolute ethanol:0.2mol·L^(-1) citric acid solution(7∶3)as the extraction solvent,and the single factor experiment was carried out with ultra-high pressure,ultra-high pressure time and ultrasonic time as the investigation factors.The optimum extraction process was obtained by response surface optimization experiment.The results showed that the optimum extraction process of anthocyanins was as follows:the ultra-high pressure was 270MPa,the ultra-high pressure time was 1.9min,and the ultrasonic time was 8.5min.Under these conditions,the maximum extraction value of anthocyanins was 49.68mg·100g^(-1),which reached 99.31%of the theoretical predicted value.Compared with single ultrasonic extraction,this combination method increased the extraction rate by 17.80%and shortened the extraction time by 30.58%.The scavenging rates of DPPH free radical and ABTS free radical in anthocyanin extract were 57.62%,44.83%and 54.74%,42.48%,respectively.It can be seen that the combination of ultra-high pressure and ultrasonic extraction effectively improved the anthocyanin extraction rate and the scavenging capacity of DPPH free radical and ABTS free radical.Qualitative analysis and quantitative determination of anthocyanin composition in purple corn seeds were carried out by liquid chromatography-mass spectrometry(LC-MS).Twelve anthocyanins were isolated by the two extraction methods,among which the single ultrasonic extraction did not contain cyanidin-3-O-dimalonylglucoside and the combined extraction did not contain malvidin-3-O-glucoside.Among the 10 anthocyanins contained by the two extraction methods,the content of pelargonidin-3-O-malonylglucoside is the highest,and that of peonidin-3-O-glucoside is the lowest.