Study on Supercritical Fluid Extraction Process of Rosemary Natural Antioxidant
2019-09-14 07:05:00
Abstract: The natural antioxidants of rosemary were extracted by supercritical CO2 fluid extraction technology. The single factor experiment and orthogonal experimental design were used to obtain the yield. The technical parameters of Zuijia process were extraction pressure 30MPa, extraction temperature 55 °C, analysis. The pressure was 5 MPa, the analytical temperature was 70 ° C, the extraction time was 3 h, and the amount of entrainer (95% ethanol) was 40% of the charge.
Key words: supercritical CO2 fluid extraction, rosemary, natural antioxidant rosemary (Rosmarinus officinalis L.) is a plant of the genus Rosemary, a perennial evergreen shrub native to Europe, North Africa and the Mediterranean coast. In recent years, it has been planted in large areas in the south of the Yangtze River in China. Its main components are diterpenoids, flavonoids, triterpenoids and essential oils, which are widely used in food, medicine, cosmetics and daily necessities.
Dried rosemary leaves have a long history as a food spice. Modern research has shown that the non-volatile components of rosemary have significant antioxidant effects, especially their good thermal stability and non-volatility, and are widely used in the food industry for noodles, fried foods, meat and Long-term storage of edible oils.
There are many methods for extracting rosemary, such as hexane extraction, ethanol extraction, methanol extraction, acetone extraction, etc., and steam distillation and molecular distillation methods are also employed. However, some of these methods may have residual organic solvents, which are harmful to the human body, and some may not ideally control the aroma, taste and antioxidant capacity of the extract, which is unfavorable to the quality of the product.
1.1 Materials and Equipment Rosemary (Rosmarinus officinalis L.) is supplied by the Yuxi Rosemary Planting Base in Yunnan. SFE supercritical fluid extraction equipment, manufactured by Guangzhou Light Industry Research Institute.
1.2 Process Flow The rosemary powder crushed to a certain particle size is charged into the extraction kettle to heat the SFE system. When the temperature reaches the predetermined temperature, the CO2 gas cylinder is opened for gas supply. When the pressure reaches the predetermined pressure, the cycle extraction is started. 10 MPa, 40 ° C, 2 h After extracting the essential oil, adjust the temperature, pressure, flow rate again, and add a certain amount of entrainer, constant temperature and constant pressure extraction for a certain time, discharge from the analytical kettle, remove the entrainer by vacuum rotary evaporation, and obtain the extraction. Object.
2 Results and discussion
2.1 Influence of different content of entrainer Supercritical CO 2 is a non-polar solvent, similar to hexane in many respects, and has poor solubility to certain polar substances (such as flavonoids, phenols, alkaloids, etc.). The addition of a polar entrainer can adjust the polarity of supercritical CO 2 and improve the solubility of CO 2 , thereby greatly improving the extraction range of supercritical CO 2 . According to the requirements of food hygiene, 95% ethanol was used as the entrainer to study the effect of different content of entrainer on the yield of oxidant.
The results showed that when the entrainer was not used, the extraction rate was very low, only 1.64%; when the entrainer was used, the extraction rate was greatly improved, but the ratio of entrainer had a great influence on the extraction rate, and there was a proper ratio of zui, lower than Or higher than this ratio will cause the significant decrease in extraction rate mainly because on the one hand, the addition of ethanol greatly increases the polarity of supercritical CO2, enhances the solubility, and increases the extraction rate; on the other hand, excessive ethanol The extraction rate is not significantly improved, which is related to the influence of excessive ethanol on the density of CO2 and the interaction between ethanol and CO2. The experiment found that when the entrainer (95% ethanol) was 40% of the charge, the yield reached a large zui.
2.2 Selection of extraction time The results showed that the extraction rate increased with time, the effect of the first lh was not significant, and increased significantly after 2h. After 3h, it tends to balance and increase slowly, so the extraction time is 3h.
2.3 Orthogonal experiment and data analysis The supercritical C02 extraction process is affected by many factors, such as extraction pressure, temperature, analytical pressure, temperature, presence or absence of entrainer and entrainer, flow rate of CO 2 , particle size of sample, morphology and many more. According to the pre-experiment results and equipment, it is decided to use 95% ethanol as the entrainer. The dosage is 40% of the charge, the extraction time is 3h, and the CO2 flow rate is set to l2L/1l. Therefore, in the orthogonal experiment, four main factors of extraction pressure (A), extraction temperature (B), analytical pressure (C) and analytical temperature (D) were designed. Four orthogonal experiments were designed to determine the comparison. Excellent supercritical CO2 fluid extraction process parameters of rosemary natural antioxidants. It can be seen from the table that the order of the four factors affecting the yield is: analytical pressure > extraction pressure > analytical temperature > extraction temperature.
3 Conclusion
3.1 The four factors affect the extraction rate in the order of magnitude: Analytical Pressure > Extraction Pressure > Analytical Temperature > Extraction Temperature.
3-2 The presence or absence of entrainer has a great influence on the yield. The use of entrainer can significantly increase the yield, but not as much as possible, but the increase is not obvious. This study shows that the use of 95% ethanol as the entrainer is 40% of the charge.
3.3 From the results of orthogonal experiment and single factor experiment, we can see that the yield of the supercritical CO2 fluid extraction of rosemary antioxidant is as follows: extraction pressure 30MPa, extraction temperature 55 °C, analytical pressure 5MPa, analytical temperature 70 ° C, extraction time 3h, entrainer (95% ethanol) dosage is 40% of the loading.
references:
[l] Tu Pengfei, Xu Zhanhui. The chemical composition of the new resource plant rosemary and its application [J]. Natural Product Research and Development, 1998, l0(3): 62-68.
[2] Yang Yan. The nature and application of rosemary extract [J]. China Food Industry, 1999, 6(3): 38-39
Key words: supercritical CO2 fluid extraction, rosemary, natural antioxidant rosemary (Rosmarinus officinalis L.) is a plant of the genus Rosemary, a perennial evergreen shrub native to Europe, North Africa and the Mediterranean coast. In recent years, it has been planted in large areas in the south of the Yangtze River in China. Its main components are diterpenoids, flavonoids, triterpenoids and essential oils, which are widely used in food, medicine, cosmetics and daily necessities.
Dried rosemary leaves have a long history as a food spice. Modern research has shown that the non-volatile components of rosemary have significant antioxidant effects, especially their good thermal stability and non-volatility, and are widely used in the food industry for noodles, fried foods, meat and Long-term storage of edible oils.
There are many methods for extracting rosemary, such as hexane extraction, ethanol extraction, methanol extraction, acetone extraction, etc., and steam distillation and molecular distillation methods are also employed. However, some of these methods may have residual organic solvents, which are harmful to the human body, and some may not ideally control the aroma, taste and antioxidant capacity of the extract, which is unfavorable to the quality of the product.
1.1 Materials and Equipment Rosemary (Rosmarinus officinalis L.) is supplied by the Yuxi Rosemary Planting Base in Yunnan. SFE supercritical fluid extraction equipment, manufactured by Guangzhou Light Industry Research Institute.
1.2 Process Flow The rosemary powder crushed to a certain particle size is charged into the extraction kettle to heat the SFE system. When the temperature reaches the predetermined temperature, the CO2 gas cylinder is opened for gas supply. When the pressure reaches the predetermined pressure, the cycle extraction is started. 10 MPa, 40 ° C, 2 h After extracting the essential oil, adjust the temperature, pressure, flow rate again, and add a certain amount of entrainer, constant temperature and constant pressure extraction for a certain time, discharge from the analytical kettle, remove the entrainer by vacuum rotary evaporation, and obtain the extraction. Object.
2 Results and discussion
2.1 Influence of different content of entrainer Supercritical CO 2 is a non-polar solvent, similar to hexane in many respects, and has poor solubility to certain polar substances (such as flavonoids, phenols, alkaloids, etc.). The addition of a polar entrainer can adjust the polarity of supercritical CO 2 and improve the solubility of CO 2 , thereby greatly improving the extraction range of supercritical CO 2 . According to the requirements of food hygiene, 95% ethanol was used as the entrainer to study the effect of different content of entrainer on the yield of oxidant.
The results showed that when the entrainer was not used, the extraction rate was very low, only 1.64%; when the entrainer was used, the extraction rate was greatly improved, but the ratio of entrainer had a great influence on the extraction rate, and there was a proper ratio of zui, lower than Or higher than this ratio will cause the significant decrease in extraction rate mainly because on the one hand, the addition of ethanol greatly increases the polarity of supercritical CO2, enhances the solubility, and increases the extraction rate; on the other hand, excessive ethanol The extraction rate is not significantly improved, which is related to the influence of excessive ethanol on the density of CO2 and the interaction between ethanol and CO2. The experiment found that when the entrainer (95% ethanol) was 40% of the charge, the yield reached a large zui.
2.2 Selection of extraction time The results showed that the extraction rate increased with time, the effect of the first lh was not significant, and increased significantly after 2h. After 3h, it tends to balance and increase slowly, so the extraction time is 3h.
2.3 Orthogonal experiment and data analysis The supercritical C02 extraction process is affected by many factors, such as extraction pressure, temperature, analytical pressure, temperature, presence or absence of entrainer and entrainer, flow rate of CO 2 , particle size of sample, morphology and many more. According to the pre-experiment results and equipment, it is decided to use 95% ethanol as the entrainer. The dosage is 40% of the charge, the extraction time is 3h, and the CO2 flow rate is set to l2L/1l. Therefore, in the orthogonal experiment, four main factors of extraction pressure (A), extraction temperature (B), analytical pressure (C) and analytical temperature (D) were designed. Four orthogonal experiments were designed to determine the comparison. Excellent supercritical CO2 fluid extraction process parameters of rosemary natural antioxidants. It can be seen from the table that the order of the four factors affecting the yield is: analytical pressure > extraction pressure > analytical temperature > extraction temperature.
3 Conclusion
3.1 The four factors affect the extraction rate in the order of magnitude: Analytical Pressure > Extraction Pressure > Analytical Temperature > Extraction Temperature.
3-2 The presence or absence of entrainer has a great influence on the yield. The use of entrainer can significantly increase the yield, but not as much as possible, but the increase is not obvious. This study shows that the use of 95% ethanol as the entrainer is 40% of the charge.
3.3 From the results of orthogonal experiment and single factor experiment, we can see that the yield of the supercritical CO2 fluid extraction of rosemary antioxidant is as follows: extraction pressure 30MPa, extraction temperature 55 °C, analytical pressure 5MPa, analytical temperature 70 ° C, extraction time 3h, entrainer (95% ethanol) dosage is 40% of the loading.
references:
[l] Tu Pengfei, Xu Zhanhui. The chemical composition of the new resource plant rosemary and its application [J]. Natural Product Research and Development, 1998, l0(3): 62-68.
[2] Yang Yan. The nature and application of rosemary extract [J]. China Food Industry, 1999, 6(3): 38-39
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