Eucalyptus citriodora aromatic oil distillation extraction method

Abstract

The invention belongs to the technical field of aromatic oil extraction, and discloses an eucalyptus citriodora aromatic oil distillation extraction method, which comprises the following steps: pretreating eucalyptus citriodora leaves, bottling sample leaves according to a material-liquid ratio of 1: 1.6, distilling after bottling, setting the distillation time to be 1 hour, standing for 10 minutes after the distillation is completed, and separating to obtain crude oil after oil-water separation, and finally, adding anhydrous sodium sulfate into the crude oil to obtain the aromatic essential oil. According to the method disclosed by the invention, the yield of the essential oil can be effectively improved by controlling the optimal material-liquid ratio before distillation and controlling the optimal set time of distillation, so that the method for extracting the plant aromatic oil through steam distillation is optimized, and the method is suitable for extracting the lemon eucalyptus leaf aromatic oil.

Description

Technical Field

[0001] The present invention relates to the technical field of aromatic oil extraction, and particularly relates to a method for distilling and extracting lemon eucalyptus aromatic oil. Background Art

[0002] Steam distillation is a traditional method for extracting plant aromatic oil, which has the advantages of simple equipment, convenient operation, high yield, etc. Existing research shows that most of the lemon eucalyptus volatile oil has been extracted within 0 - 1 hour of lemon eucalyptus, and only some components are distilled out within 1 - 2 hours. The main component of lemon eucalyptus leaf oil, citronellal, decreases relatively with the increase of distillation time.

[0003] From the perspective of smell, the aromatic oil extracted by the existing distillation method has a relatively plain aroma and contains a certain amount of water and impurities. Therefore, the present invention proposes a method for distilling and extracting lemon eucalyptus aromatic oil to optimize the existing distillation method and improve the quality and stability of the aromatic oil. Summary of the Invention

[0004] The present invention aims to provide a method for distilling and extracting lemon eucalyptus aromatic oil to optimize the distillation method of the existing technology and improve the quality and stability of the aromatic oil.

[0005] To achieve the above purpose, the present invention provides the following technical solutions:

[0006] A method for distilling and extracting lemon eucalyptus aromatic oil, comprising the following steps:

[0007] S1. Take the fresh lemon eucalyptus leaves from the upper, middle, and lower layers of the branches of the lemon eucalyptus plant, separate the branches and leaves of the taken fresh lemon eucalyptus leaves, mix the leaves evenly and cut them into pieces, and seal them in a sealed bag and put them in a 4°C refrigerator for storage;

[0008] S2. Weigh the required sample leaves according to the solid-liquid ratio of 1:1.6 and calculate the required amount of water, and put the sample leaves and the required water into a flask together;

[0009] S3. Assemble a 500ml / 5ml tetrafluoro piston volatile oil detector and a 500mm spherical condenser from bottom to top. After assembly, carry out distillation, and control the distillation time to 1 hour;

[0010] S4. After distillation, the cooling and standing time is 10 minutes. After the oil-water separation, use a 500ml / 5ml tetrafluoro piston volatile oil detector for oil-water separation, and take out the upper liquid to obtain the crude oil;

[0011] S5. Add 2 - 3g of anhydrous sodium sulfate to dehydrate the crude oil part to obtain lemon eucalyptus aromatic oil.

[0012] Further, in step S1, the leaves are cut into pieces with a size of 1 - 2 cm 2 in size.

[0013] Further, in step S2, the amount of sample leaves is 100 g and the required amount of water is 160 ml.

[0014] Further, in step S3, when assembling the condenser tube, the rubber tube is assembled with the water inlet at the bottom and the water outlet at the top, which is convenient for giving full play to the condensation effect.

[0015] Further, in step S4, the specific operation of oil-water separation is as follows: Rotate the tetrafluoro piston, use a glass test tube to collect distilled water, immediately close the tetrafluoro piston before the oil is almost extracted, and pour out the water in the condenser tube; Repeat the operation for extraction.

[0016] The beneficial effects of the technical solution are as follows: By controlling the optimal material-liquid ratio before distillation and the optimal set time of distillation, this method can effectively improve the extraction rate of essential oil, thereby improving the stability of obtaining aromatic oil and the quality of the obtained aromatic oil; The present invention optimizes the traditional distillation method and obtains the optimal distillation extraction method of Eucalyptus citriodora Hook. oil by controlling the optimal material-liquid ratio and the optimal distillation time. Description of the Drawings

[0017] Figure 1 It is the distillation process flow chart of the method of the present invention;

[0018] Figure 2 It is the essential oil yield corresponding to different extraction times in the embodiment of the present invention;

[0019] Figure 3 It is the essential oil yield corresponding to different material-liquid ratios in the embodiment of the present invention; Detailed Embodiments

[0020] The present invention will be further described in detail below with reference to the drawings and embodiments:

[0021] As Figure 1 shown is the flow chart of a method for distilling and extracting Eucalyptus citriodora Hook. oil of the present invention.

[0022] Embodiment

[0023] Experimental supplies: Pure water, anhydrous sodium sulfate, sample leaves. Among them, the sample leaves are taken from healthy adult Eucalyptus citriodora Hook. plants, and the mature fresh leaves from the upper, middle, and lower layers of the branches are collected and mixed evenly. The collected fresh Eucalyptus citriodora Hook. sample leaves are separated from the branches and leaves, and after the leaves are mixed evenly, each leaf is cut to 1-2 cm 2 in size, and then sealed with a sealed bag and refrigerated in a 4°C refrigerator.

[0024] Experimental instruments: Carbon fiber tree sampler, Test electronic temperature-controlled magnetic stirring digital display electrothermal mantle, 500 mm spherical condenser, 500 ml / 5 ml tetrafluoro piston volatile oil determination device, 2 m yellow rubber tube, 1000 ml round-bottom flask, plastic dropper, 500 ml measuring cylinder, electronic balance, 7890-7000 gas chromatography-triple quadrupole mass spectrometer.

[0025] Design two single-factor experiments on extraction time and solid-liquid ratio. Set the extraction times to three treatments of 1 h, 1.5 h, and 2 h, and set the solid-liquid ratios to 1:1.6, 1:1.8, and 1:2.0 (as shown in Table 1). Study the effects of extraction time and solid-liquid ratio on the oil yield of lemon leaf essential oil, explore the optimal extraction process of lemon leaf essential oil, set 3 replicates for each experiment, and take the average value of the final results.

[0026] Table 1 Design of process factors and levels for steam distillation

[0027]

[0028] Experimental operation process:

[0029] Take out the pre-treated and preserved sample leaves from the 4°C refrigerator, weigh them on the balance according to the solid-liquid ratio to calculate the required weight, and its mass is m1.

[0030] Control the solid-liquid ratios to 1:1.6, 1:1.8, and 1:2.0 respectively, and put the sample leaves into a 1000 ml round-bottom flask.

[0031] Assemble the 500 ml / 5 ml tetrafluoro piston volatile oil determination device and the 500 mm spherical condenser from top to bottom in sequence. After assembly, carry out distillation.

[0032] Control the distillation times to 1 h, 1.5 h, and 2.0 h respectively, and adjust the temperature of the electronic temperature-controlled magnetic stirring digital display electrothermal mantle to 100°C to boil.

[0033] After distillation, the cooling and standing time is 10 min. After the oil-water separation, use the 500 ml / 5 ml tetrafluoro piston volatile oil determination device for oil-water separation. The specific operation is as follows: Rotate the tetrafluoro piston, collect distilled water with a glass test tube, immediately close the tetrafluoro piston before the oil is about to be extracted, and pour out the water in the condenser; repeat the operation to obtain crude oil.

[0034] Add 2-3 g of anhydrous sodium sulfate to dehydrate the oil-water mixture part of the crude oil; place the glass bottle on the balance and record the value m2, use a plastic dropper to collect the remaining essential oil sample, and transfer it to an empty bottle for secondary weighing and record the value m3.

[0035] The calculation formula for the oil yield is: (m3 - m2) / m1 × 100%, where m1 is the total mass of the sample leaves, m2 is the total mass of the sample, and m3 is the net mass of the essential oil.

[0036] According to the above experimental process, weigh the fresh Eucalyptus citriodora leaves at 100 g per portion, and use a 500 ml graduated cylinder to separately take 160 ml, 180 ml, and 200 ml of ultrapure water according to the set solid-liquid ratio, and conduct single-factor experiments successively according to the distillation times of 1 h, 1.5 h, and 2 h. Conduct 3 parallel experiments for each group, and finally obtain the average oil yield, with a total of 9 groups of data and 9 average oil yield values. (See Table 2)

[0037] Table 2 Experimental results of extracting Eucalyptus citriodora essential oil by steam distillation

[0038]

[0039] Result analysis:

[0040] Effect of extraction time on the essential oil yield

[0041] Under the condition that the solid-liquid ratio and all test factors are the same, the effects of different extraction times on the essential oil yield are as Figure 2 shown. It can be seen from the figure that with the extension of the extraction time, there are obvious differences in the essential oil yields of Eucalyptus citriodora leaves with different solid-liquid ratios. When the extraction time is 1 h, the oil yield is the highest when the solid-liquid ratio is 1:1.6 and the lowest when it is 1:1.8; however, with the extension of the extraction time, the oil yield of the solid-liquid ratio of 1:1.6 will gradually decrease, while the oil yields of the solid-liquid ratios of 1:1.8 and 1:2.0 both increase with the increase of time.

[0042] Effect of solid-liquid ratio on the essential oil yield

[0043] Under the condition that the extraction time and other test factors are the same, the effects of different solid-liquid ratios on the essential oil yield are as Figure 3 shown. When the solid-liquid ratio is 1:1.6, the oil yield is the highest when extracted for 1 h and the lowest when extracted for 2 h; when the solid-liquid ratios are 1:1.8 and 1:2.0, the oil yields are the highest when extracted for 2 h and the lowest when extracted for 1 h.

[0044] The results of this experiment show that when the material-liquid ratio is 1:1.6, the average oil yield decreases with the increase of time; when the material-liquid ratio is 1:1.8 and 1:2.0, the average oil yield increases with the increase of time, and the highest value of the average oil yield is 1.1612%. According to the existing technical theory, most of the volatile oil in Eucalyptus citriodora has been extracted within 0-1.0 h, and only some of the post-components are distilled out within 1.0-2.0 h. In order to reduce the relative energy consumption, it is more appropriate to control the distillation time of Eucalyptus citriodora leaves at 1.0 h. Therefore, when the distillation time is fixed, it is determined that the material-liquid ratio of 1:1.6 and the distillation time of 1 h are the optimal extraction conditions for extracting the essential oil from Eucalyptus citriodora leaves by the steam distillation method.

[0045] The above are only examples of the present invention, and specific technical solutions or common knowledge such as characteristics known in the solutions are not described in detail herein. It should be noted that for those skilled in the art, without departing from the technical solution of the present invention, several deformations and improvements can still be made, which should also be regarded as the protection scope of the present invention, and these will not affect the implementation effect of the present invention and the practicality of the patent. The protection scope required by this application should be based on the content of its claims, and the specific implementation manners described in the specification can be used to explain the content of the claims.

Claims

1. A method for distilling and extracting lemon eucalyptus aromatic oil, characterized in that, It includes the following steps: S1 Take the fresh Eucalyptus citriodora leaves from the upper, middle, and lower layers of the branches of Eucalyptus citriodora plants. Separate the branches and leaves of the taken fresh Eucalyptus citriodora leaves. After mixing the leaves evenly, cut them into pieces, seal them with a sealed bag, and put them in a refrigerator at 4°C for storage; S2 Weigh the required sample leaves according to the solid-liquid ratio of 1:1.6 and calculate the required amount of water. Put the sample leaves and the required water into a flask together; S3 Assemble a 500 ml / 5 ml tetrafluoro piston volatile oil detector and a 500 mm spherical condenser in sequence from bottom to top. After the assembly is completed, carry out distillation, and control the distillation time to 1 h; S4 After distillation, the cooling and standing time is 10 min. After the oil and water are separated, use a 500 ml / 5 ml tetrafluoro piston volatile oil detector to separate the oil and water, and take out the upper liquid to obtain the crude oil; S5 Add 2 - 3 g of anhydrous sodium sulfate to dehydrate the crude oil part to obtain Eucalyptus citriodora aromatic oil.

2. The method for distilling and extracting lemon eucalyptus aromatic oil according to claim 1, wherein: In the step S1, the leaves are cut to 1-2 cm in size. 2 Size.

3. A method for distilling and extracting lemon eucalyptus aromatic oil according to claim 1, characterized in that: In step S2, the amount of sample leaves is 100 g, and the required amount of water is 160 ml.

4. A method for distilling and extracting lemon eucalyptus aromatic oil according to claim 1, characterized in that: In step S3, when assembling the condenser, the assembly of the rubber tube is from bottom to top for water inlet and from top to bottom for water outlet, which is convenient to fully exert the condensation effect.

5. A method for distilling and extracting lemon eucalyptus aromatic oil according to claim 1, characterized in that, The specific operation of oil-water separation in step S4 is as follows: Rotate the tetrafluoro piston, use a glass test tube to collect distilled water, immediately close the tetrafluoro piston immediately before the oil is about to be extracted, and pour out the water in the condenser; Repeat the operation for extraction.

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