The ultrasonic-assisted extraction technology of the bergamot essential oil
Abstract: The method of ultrasonic-assisted steam distillation for extraction of essential oil from bergamot was studied by using bergamot as raw material. The optimum technological conditions were as follows: water distillation flow was 1.30 mL / min, ultrasonic power was 180 W, auxiliary working time was 30 min, and steam distillation time was 75 min. Under this condition, the extraction rate of essential oil from bergamot was 0.763%. Key words: Buddha fruit; essential oil; ultrasonic assisted
Bergamot (Bergamot) is Rutaceae oranges citrus variants, as evergreen small trees [1]. The bergamot fruit is golden, fleshy and tender, crisp and sweet, except for fresh food, can be made candied fruit, preserved fruit, and processed into bergamot tea, bergamot, bergamot jelly and bergamot wine, its flowers, young fruit and Mature fruit can be used as medicine [2]. Fructus fruit essential oil contains mainly aldehydes, mono-olefins, monoterpene alcohols, esters, furan coumarin, etc. [3-4].
Bergamot essential oil extraction methods are mainly steam distillation, organic solvent extraction, cold pressing and supercritical CO 2 extraction [5-6]. Water vapor distillation is widely used in plant essential oil extraction because of its simple equipment, low cost and high yield. In this experiment, Ultrasonic-assisted steam distillation was used to extract the essential oil from the bergamot, which provided the scientific basis for the extraction and application of the essential oil.
1. experimental part
1.1 Instruments and drugs
KQ-300DE medical ultrasonic ultrasonic cleaner (ultrasonic frequency (KHz) 40, ultrasonic power (W) 300): Kunshan City ultrasound Instrument Co., Ltd.; KDM-type thermostat: ChangSha Plantat Natural Ingredients Inc.; 101A- TU-1900 dual-beam UV visible spectrophotometer: Beijing Pu analysis of general equipment limited liability company; FA2104 electronic balance, 752N-type UV-visible spectrophotometer : Shanghai Precision Science Instrument Co., Ltd.
Bergamot fruit: picking in Guangdong Ji Gong Health Food Co., Ltd. planting base, cut into 4 mm small spare. The chemical reagents used are analytical grade, provided by Chaozhou Chemical Reagent Company.
1.2 Experimental steps
1.2.1 Spectral characteristics of bergamot essential oil The extracted Fructus balsamus oil was dissolved in dichloromethane and the solution was scanned with a TU-1900 dual-beam UV-Vis spectrophotometer in the wavelength range of 200-600 nm to obtain the spectral characteristics of the essential oil The
1.2.2 The relationship between the content of essential oil and absorbance of the study of fresh fruit from the bergamot, steam distillation method for 1.5 h, extracted with dichloromethane 2 times (5 mL × 2), combined extract. Remove the essential oil extract 0.00,0.10,0.20,0.30,0.40,0.50 mL, with two
Chloride was set at 10 mL, and the absorbance was measured at the characteristic absorption peak (235 nm) of essential oil. The volume fraction was taken as the abscissa, and the absorbance was plotted as the ordinate. The relationship between the essential oil content and the absorbance was investigated.
1.2.3 Extraction process optimization (1) Comparison of extraction methods: Weigh two fresh fruit bergamot, each 50 g, respectively, using steam distillation and ultrasonic-assisted steam distillation distillation 1.5 h; where the ultrasonic power of 180 W, the auxiliary time is 30 min; extracted twice with methylene chloride (5 mL × 2), the combined extract, to be tested.
(2) Optimization of extraction process by ultrasonic assisted steam distillation
(A) Distillation time: 7 parts of fresh fruit, 50 g each, with ultrasonic-assisted steam distillation method were distilled 15,30,45,60,75,90,105 min, ultrasonic power of 180 W, ultrasonic assisted time For 30 min, extracted twice with methylene chloride (5 mL x 2), combined with the extract, to be tested.
(B) the choice of ultrasonic power: weighed 6 fresh fruit bergamot, each 50 g, ultrasonic-assisted steam distillation distillation 75 min, the auxiliary time of 30 min, the role of power were 120,150, 180,210,240, 270 W, extracted twice with methylene chloride (5 mL x 2), combined with the extract, to be tested.
(C) the auxiliary time of ultrasonic: Weigh the bergamot fruit 5 copies, each 50 g, with ultrasonic-assisted steam distillation distillation 75 min, ultrasonic power of 180 W, the auxiliary time were 15,25,30,35,45 min, extracted twice with methylene chloride (5 mL × 2), the combined extract, to be tested. Take the above extraction solution 0.30 mL, with methylene chloride volume to 10 mL, in the essential oil absorption peak (235 nm) measured its absorbance. The above process is optimized for each experiment. Three of the experiments are parallel, and the data are the average of the three experimental results.
1.2.4 Verification experiment of extraction process of bergamot essential oil In the experiment, 120 g of bergamot fruit was distilled, distilled by steam-assisted distillation for 75 min, ultrasonic power was 180 W, auxiliary time was 30 min, extracted twice with dichloromethane (12 ML x 2). The extracts were combined. The dichloromethane was distilled off and dried at 40 ° C. The yield was calculated and the yield was calculated. The experimental data were arranged in three groups, and the listed data were the average of the three experimental results.
2 Results and analysis
2.1 Spectral characteristics of brucella essential oil
In the wavelength range of 200 ~ 600 nm, the bergamot oil is scanned, the obtained spectrum shown in Figure 1. It can be seen from Figure 1, the Buddha fruit oil in the UV area at 235 nm at the maximum absorption peak.
Figure 1: bergamot oil Spectral curve
2.2 The relationship between the content of essential oil and the absorbance function
Figure 2：Bergamot essential oil Volume fraction versus Absorbance relationship
According to the experimental method in Section 1.2.2, the volume fraction of the extracts of the bergamot oil extract is between 0.00 and 5.00%. The absorbance of each solution is measured at 235 nm. According to the experimental data, From Figure 2
It can be seen that the volume fraction of the essential oil extract has a good proportional relationship with the absorbance, and the linear relationship between the two is: A = 0.1185φ; R2 = 0.9962. Indicating that the bergamot oil methylene chloride solution absorbance in the range of 0 to 0.7, the absorbance can be used as the basis for judging the content of essential oils.
2.3 Optimization of extraction process
(1) Optimization of distillation method: The experimental results show that the absorbance of ultrasonic-assisted steam distillation and steam distillation extraction under the same temperature and time are compared with those of steam distillation and ultrasonic-assisted steam distillation. 0.568, 0.501, ultrasonic assisted steam distillation of the extraction efficiency is higher.
(2) Optimization of extraction process by ultrasonic assisted steam distillation: (A) Selection of distillation time, fixed ultrasonic assisted working power and action time, and the effects of steam distillation time and water vapor on extraction efficiency were investigated. The data are shown in Table 1
From Table 1, it can be seen that the evapotranspiration of bruxine essential oil increased with the increase of time. The absorbance of the extract increased with the increase of time, and the absorbance increased obviously 75 min before distillation. After 75 min, the absorbance increased with time The change was not obvious, indicating that the steam flow was about 1.30 mL / min, the ultrasonic assisted distillation was 75 min, and the fresh fruit of the bergamot was distilled off. (B) the choice of ultrasonic power: fixed distillation flow of about 1.30 mL / min, distillation time 75 min, ultrasonic auxiliary effect 30 min, to study the ultrasonic power changes on the extraction efficiency of brucella fruit oil, the experimental results shown in Figure 3.
Figure 3: The relationship between Ultrasonic power and Extraction efficiency
It can be seen from Figure 3, with the ultrasonic power increases, the extraction efficiency of the first increase after the trend of decline, the power is 180W when the extreme value. (C) Ultrasonic auxiliary time selection: fixed distillation flow of 1.30 mL / min, distillation time 75 min, ultrasonic power 180 W, to study the ultrasonic assisted time on the extraction efficiency of essential oils, the experimental data shown in Figure 4.
Figure 4 The relationship between Ultrasonic assisted time and Extraction efficiency
Figure 4 results show that when ultrasound is assisted
Between 30 min, the highest extraction efficiency of essential oils. The optimized process of ultrasonic distillation of bergamot oil is 1.30 mL / min, the power of ultrasonic is 180 W, the working time is 30 min, and the distillation time is 75 min.
2.4 Verification experiment of extraction of essential oil from Buddha fruit
Weigh the bergamot fruit 120 g, according to the optimized ultrasonic assisted steam distillation method to extract essential oil, dry fruit and fruit oil 0.9156 g, the extraction rate of 0.763%
3 Conclusion
The essential oil has a strong absorption peak at 235 nm, and the content of essential oil in dichloromethane has a good linear correlation with the absorbance. The single factor experiment was used to extract the essential oil
The optimum technological conditions were as follows: the water distillation flow was 1.30 mL / min, the ultrasonic power was 180 W, the auxiliary working time was 30 min, and the distillation time was 75 min. Under these conditions, the yield of essential oil from bergamot was 0.763%.
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