Weiyan Luo,Yixin Chen,Ping Hu,Wei Ruan,Yueyuan Ye,Zhifeng Zheng,Shuirong Li,Dechao Wang,Duo Wang
A heterogeneous extracting route of 4-ethylguaiacol is constructed using the intermediate of the reaction between 4-ethylguaiacol and Ca 2+ as the extracting agent. In this work, 4-ethylguaiacol with different concentrations (70, 80, 90, 95%) is prepared using 40 v/v% ethanol aqueous solution as the mother liquor. The extraction parameters optimization, cycle extraction and 4-ethylguaiacol purification are studied, respectively. Extracting parameters investigated are reaction temperature (4–80 ℃), extraction time (5–60 min), and pH value (6.5–13). 4-ethylguaiacol extraction efficiency keeps above 90% at the optimum extracting conditions at the reaction temperature of 4–20 ℃, the extraction time of 30 min, and the pH value of 6.5–10. Further cycle extraction experiments are carried out under the optimal extraction parameters using the intermediate as the extracting agent. After 36 cycle extraction times, the extraction efficiency of 4-ethylguaiacol can still reach 91.7%. Guaiacol has similar physical and chemical properties to 4-ethylguaiacol, thus it is used as an impurity to test the extraction and purification effect of the heterogeneous extracting method. With increasing the cycle extraction times from 1 to 4, 4-ethylguaiacol purity reaches more than 99% for all four mother liquors with different initial concentrations. 4-ethylguaiacol purity of 99.57% is achieved through twice cycle extraction when its initial content in the mother liquor is 95%.
Fengli Chen,Qiang Zhang,Shimin Fei,Huiyan Gu,Lei Yang
In this study, ultrasonic circulating extraction (UCE) technique was firstly and successfully applied for extraction of samara oil from Acer saccharum . The extraction kinetics were fitted and described, and the extraction mechanism was discussed. Through comparison, n -hexane was selected as the extraction solvent, the influence of solvent type on the responses was detailedly interpreted based on the influence of their properties on the occurrence and intensity of cavitation. Seven parameters potentially influencing the extraction yield of samara oil and content of nervonic acid, including ultrasound irradiation time, ultrasound irradiation power, ultrasound temperature, liquid-solid ratio, soaking time, particle size and stirring rate, were screened through Plackett–Burman design to determine the significant variables. Then, three parameters performed statistically significant, including liquid-solid ratio, ultrasound irradiation time and ultrasound irradiation power, were further optimized using Box–Behnken design to predict optimum extraction conditions. Satisfactory yield of samara oil (11.72 ± 0.38%) and content of nervonic acid (5.28 ± 0.18%) were achieved using the optimal conditions. 1% proportion of ethanol in extraction solvent, 120 °C of drying temperature and 6.4% moisture were selected and applied for effective extraction. There were no distinct differences in the physicochemical properties of samara oil obtained by UCE and Soxhlet extraction, and the samara oil obtained by UCE exhibited better antioxidant activities. Therefore, UCE method has enormous potential for efficient extraction of edible oil with high quality from plant materials.