CN110655989A - Method for extracting and separating volatile oil and aromatic water from houttuynia cordata - Google Patents
Method for extracting and separating volatile oil and aromatic water from houttuynia cordata Download PDFInfo
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Abstract
The invention provides a method for extracting and separating volatile oil and saturated aromatic water from houttuynia cordata, which comprises the following steps: a primary distillation stage: distilling the houttuynia cordata by first steam to obtain primary distilled steam; performing primary distillation condensation I, primary distillation condensation II, primary distillation oil-water separation I and primary distillation oil-water separation II on the primary distillation steam to respectively obtain primary distillation liquid and volatile oil; a redistillation stage: distilling the primary distilled liquid obtained by the primary distillation with second steam to obtain redistilled steam; carrying out redistillation condensation I, redistillation condensation II and redistillation oil-water separation on the redistilled steam to respectively obtain saturated aromatic water and volatile oil; wherein in the primary distillation, the temperature of the primary distillation liquid is controlled to be not more than 40 ℃ and more than the freezing point of the primary distillation liquid; and in the redistillation, controlling the temperature of the saturated aromatic water to be not more than 30 ℃ and to be more than the freezing point of the saturated aromatic water.
Description
Technical Field
The invention relates to a method for extracting volatile oil and aromatic water from houttuynia cordata, and belongs to the field of traditional Chinese medicine extraction.
Background
The traditional method for extracting volatile oil and aromatic water from houttuynia cordata generally comprises the steps of separately extracting the volatile oil and the aromatic water.
The common methods for extracting volatile oil and aromatic water from herba Houttuyniae include steam distillation, solvent method, and critical extraction.
The steam distillation method has the characteristics of simple equipment, safe operation, no environmental pollution, low cost, avoidance of influence of organic solvent residue on oil quality in the extraction process and the like, is more suitable for industrial mass production than other methods, is an important method for effectively extracting the traditional Chinese medicine volatile oil, and is also a volatile oil extraction formula specified in pharmacopoeia.
The method for extracting the volatile oil from the houttuynia cordata is a reflux extraction method recorded in the appendix of the four parts of the Chinese pharmacopoeia 2015 edition. In the method, steam generated by an extraction tank is subjected to primary condensation and primary oil-water separation, the obtained condensate flows back to a distillation tank, and then reflux extraction is repeatedly carried out for 5-10 hours. After extraction, discharging the upper layer volatile oil from oil-water separator.
In the method, the condensate flows back to the distillation retort, and the volatile oil can be obtained only by repeated high-temperature heating distillation. The method does not control the distillation temperature in the distillation process, and the effective components in the volatile oil are easy to decompose due to long-time heating. The volatile oil obtained by the method is dark in color and is yellow or reddish brown, which indicates that partial components in the volatile oil are decomposed. And the method only has primary condensation and primary oil-water separation. Under the condition that the condensate is at a higher temperature and only has primary oil-water separation, the cooling of the condensate and the oil-water separation of the condensate cannot be completely carried out, and further the yield of the volatile oil extracted from the houttuynia cordata is low.
Disclosure of Invention
The invention aims to provide a high-quality and high-efficiency method for extracting and separating volatile oil and saturated aromatic water from houttuynia cordata.
The invention provides a method for extracting and separating volatile oil and saturated aromatic water from houttuynia cordata, which comprises the following steps:
a primary distillation stage: distilling the houttuynia cordata by first steam to obtain primary distilled steam; performing primary distillation condensation I, primary distillation condensation II, primary distillation oil-water separation I and primary distillation oil-water separation II on the primary distillation steam to respectively obtain primary distillation liquid and volatile oil;
a redistillation stage: distilling the primary distilled liquid obtained by the primary distillation with second steam to obtain redistilled steam; carrying out redistillation condensation I, redistillation condensation II and redistillation oil-water separation on the redistilled steam to respectively obtain saturated aromatic water and volatile oil;
wherein in the primary distillation, the temperature of the primary distillation liquid is controlled to be not more than 40 ℃ and more than the freezing point of the primary distillation liquid; and in the redistillation, controlling the temperature of the saturated aromatic water to be not more than 30 ℃ and to be more than the freezing point of the saturated aromatic water.
In the primary distillation stage, the temperature of the primary distillation liquid is controlled by adjusting the pressure of the first steam, the temperature of the condensed water in the primary distillation condensate I and the temperature of the condensed water in the primary distillation condensate II.
The pressure of the first steam is 0.04-0.1 MPa; preferably, the pressure of the first steam is 0.04-0.08 MPa.
The temperature of cooling water in the primary distillation condensation I is 5-20 ℃; preferably, the temperature of the cooling water in the preliminary distillation condensation I is 6-18 ℃.
The temperature of cooling water in the primary distillation condensation II is 20-30 ℃; preferably, the temperature of the cooling water in the preliminary distillation condensation II is 22-28 ℃.
And regulating and controlling the temperature of the saturated aromatic water by regulating the pressure of the second water vapor, the temperature of the condensed water in the redistillation condensation I and the temperature of the condensed water in the redistillation condensation II.
The pressure of the second steam is 0.04-0.1 MPa; preferably, the pressure of the second steam is 0.04-0.08 MPa.
The temperature of cooling water in the redistillation condensation I is 0-10 ℃; preferably, the temperature of the cooling water in the redistillation condensate I is 0 to 8 ℃.
The temperature of cooling water in the redistillation condensation II is 20-30 ℃; preferably, the temperature of the cooling water in the redistillation condensate II is 22 to 28 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention combines the processes of extracting volatile oil from the houttuynia cordata and extracting saturated aromatic water from the houttuynia cordata, optimizes the processes, simplifies the production process and improves the production efficiency.
2. The invention adopts primary distillation secondary condensation and secondary distillation condensation (chilled water), can quickly and fully cool the distillate, reduces the damage influence of long-time high temperature on effective components in the distillate, improves the oil-water separation effect, and ensures the product quality of the final product injection.
3. The invention adopts the direct distillation method, omits the reflux process, can avoid repeated high-temperature heating of the volatile oil for a long time, and prevents the damage of the effective components in the volatile oil.
4. The invention adopts primary distillation secondary oil-water separation to aggravate distillation primary oil-water separation, can thoroughly separate oil from water, improves the oil-water separation effect, ensures the product quality of the final product injection, and improves the yield of the volatile oil and the yield of the injection.
5. The invention controls the temperature of the distillate to keep the distillate at a lower temperature so as to further ensure the oil-water separation effect. And the extraction process can be stable and consistent through temperature control and adjustment, and finally the batch consistency of the product is good.
Drawings
FIG. 1 is a schematic diagram of a device for extracting and separating volatile oil and saturated aromatic water from houttuynia cordata according to the present invention. The device comprises a multifunctional extraction tank 1, a primary condenser I2, a secondary condenser I3, a primary oil-water separation I4, a secondary oil-water separation I5, a primary distillation liquid storage tank 6, a delivery pump 7, a heavy distillation tank 8, a primary condenser II9, a secondary condenser II10, a primary oil-water separation II11, a liquid storage tank 12, a temperature controller I13, a temperature controller II14, an elbow pipe I15, an elbow pipe II16, an elbow pipe III17, a heating steam pipeline I18, a heating steam pipeline II19, a pressure controller 20, a heating steam pipeline III21, a pressure controller 22, a liquid level controller I23 and a liquid level controller II 24.
Fig. 2 is a control fingerprint in the system for evaluating chromatographic fingerprint similarity of traditional Chinese medicines (2009 edition) with methyl-n-nonanone as a reference. In the figure, R11 corresponds to the fingerprint of methyl-n-nonanone.
Fig. 3 is a fingerprint of 16 batches of saturated aromatic water prepared in example 1. In the figure, R11 corresponds to the fingerprint of methyl-n-nonanone, and S2(11) to S17(11) correspond to the batch fingerprints of 16 batches of saturated aromatic water with the batch numbers of K100901-K100916 prepared in example 1, respectively.
Fig. 4 is a fingerprint of saturated aromatic water prepared in example 1, comparative example 1 and comparative example 2. Wherein S1 corresponds to the fingerprint of the saturated aromatic water prepared in example 1, S2 corresponds to the fingerprint of the saturated aromatic water prepared in comparative example 1, and S3 corresponds to the fingerprint of the saturated aromatic water prepared in comparative example 2.
FIG. 5 is a photograph of the volatile oil prepared in comparative example 1.
FIG. 6 is a photograph of the volatile oil prepared in comparative example 2.
Fig. 7 is a photograph of the saturated aromatic water prepared in comparative example 3.
FIG. 8 is a photograph of the volatile oil prepared in comparative example 4.
FIG. 9 is a photograph of the volatile oil prepared in comparative example 5.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the specific examples.
The invention can adopt but not limited to the device shown in figure 1 to realize the technical scheme of the invention.
The method for extracting and separating volatile oil and saturated aromatic water from houttuynia cordata comprises a primary distillation stage and a secondary distillation stage.
Wherein the specific process of the primary distillation stage is as follows: putting fresh herba Houttuyniae into multifunctional extraction tank, adding purified water, starting condensed water, introducing steam into the multifunctional extraction tank, and distilling. Steam generated by distillation in the multifunctional extraction tank passes through primary distillation condensation I and primary distillation condensation II, then passes through primary distillation oil-water separation I and primary distillation oil-water separation II, and finally enters the primary distillation liquid storage tank. When herba Houttuyniae is heated to boiling and steam is generated and condensate is distilled off, the temperature of distillate is controlled to be less than 40 deg.C by regulating steam pressure and temperature and/or fluidity of condensate to prevent decomposition of volatile oil
The primary distilled liquid obtained in the primary distillation stage can be subjected to secondary distillation stage to obtain saturated aromatic water and volatile oil. Wherein the redistillation stage comprises the following specific processes: pumping the primary distilled liquid into a heavy distillation tank, then starting cooling water and introducing steam. And (3) distilling the steam generated in the redistillation tank again to condense I and II, and then passing through a redistillation oil-water separator to obtain saturated aromatic water. And a redistillation stage, wherein the temperature of distillate is controlled to be less than 30 ℃ by adjusting the steam pressure and the temperature and flow rate of cooling water so as to prevent the decomposition of volatile oil.
After the primary distillation and the secondary distillation are finished, discharging the liquid in the oil-water separator, and taking the upper oily matter, namely the houttuynia volatile oil.
The invention detects the quality of the prepared cordate houttuynia saturated aromatic water and volatile oil according to Chinese pharmacopoeia.
The detection standard of the saturated aromatic water of the houttuynia cordata is as follows:
1. examination of traits
The product is colorless to milk white uniform suspension liquid, and has no floating, suspending or lower foreign matter; fishy smell and astringent taste.
2. pH value
The pH value of the product should be 4.0-8.0.
3. Bacterial endotoxins
Taking the product, wherein the amount of bacterial endotoxin in 1ml should be less than 0.5 EU.
4. Determination of content
Chromatographic conditions and system applicability test: a chromatographic column: DB-1 capillary column (30m × 0.25mm, 0.25 μm); temperature programming: maintaining at 70 deg.C for 5min, increasing to 140 deg.C at 5 deg.C/min, maintaining for 5min, and increasing to 250 deg.C at 20 deg.C/min; sample inlet temperature: 230 ℃; a detector: FID; detector temperature: 280 ℃; carrier gas: n2; flow rate of carrier gas: 1.0 ml/min; the split ratio is as follows: 10: 1, the theoretical plate number is more than 10000 calculated by methyl n-nonanone.
Preparing an internal standard solution: taking a proper amount of undecene, precisely weighing, adding n-hexane to prepare a stock solution of about 2mg/ml, and storing in a refrigerator.
Preparing a reference substance solution: respectively taking a proper amount of 4-terpene alcohol, d-terpineol, bornyl acetate and methyl n-nonanone reference substances, precisely weighing, adding n-hexane to prepare 10, 5, 8 and 2mg/ml stock solutions, precisely transferring 1ml, 1ml, 1ml and 5ml of the stock solutions of the reference substances into a 10ml measuring flask, and keeping the volume constant of the n-hexane in a refrigerator to serve as a mixed reference substance stock solution.
Preparing a test solution: taking 50.0ml of heartleaf houttuynia herb redistillate, placing the redistillate in a round-bottom flask, connecting with a volatile oil tester, adding water from the upper end of the tester to fill a scale part, adding 0.5ml of n-hexane, connecting with a reflux condenser tube, heating to boil, keeping slightly boiling for 40min, stopping heating, cooling to room temperature, taking an n-hexane layer, adding about 0.4g of anhydrous Na2S04, removing water, taking an upper layer solution into a measuring flask, precisely adding 0.2ml of an internal standard solution, adding n-hexane to fix the volume to 2ml, and taking the solution as a sample solution.
The determination method comprises the following steps: taking 1 μ l of each solution, injecting into a chromatograph for measurement, and calculating the content according to an internal standard method.
The product should contain 4-terpene alcohol per 1 ml: not less than 5.0. mu.g/ml, alpha-terpineol: 2.0-10.0 μ g/ml, bornyl acetate: not less than 1.0. mu.g/ml, methyl n-nonanone: 6.0-20.0 mu g/ml.
5. Finger print
Detecting according to the method under the content determination item, and recording the chromatogram.
Setting integration parameters: the first 5min solvent peak was excised, the internal standard peak was removed, Slope Sensitivity: 5; peak Width: 0.1; area reject: 4; height reject: 0.1.
the similarity is calculated by a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2009 edition), and the similarity between the fingerprint of the test sample and the fingerprint of the reference should not be lower than 0.900. The fingerprint spectrum should have 11 characteristic peaks, and the specific spectrum is shown in figure 2. Relative retention time and relative peak area of each peak are as follows, taking methyl n-nonanone as a reference peak (RT ═ 17.20 min):
| peak number | RRT | RA | Peak | RRT | RA | |
| 1 | 0.466 | 0.073 | 7 | 0.810 | 1.705 | |
| 2 | 0.487 | 0.043 | 8 | 0.828 | 0.494 | |
| 3 | 0.557 | 0.058 | 9 | 0.991 | 0.179 | |
| 4 | 0.673 | 0.053 | S | 1.000 | 1.000 | |
| 5 | 0.712 | 0.045 | 10 | 1.554 | 0.017 | |
| 6 | 0.741 | 0.037 |
Example 1
A primary distillation stage: putting the houttuynia cordata into a multifunctional extraction tank, introducing first water vapor with the pressure of 0.08MPa, and distilling to obtain primary distillation vapor; and (3) respectively obtaining primary distillation liquid and volatile oil from the primary distillation steam after primary distillation condensation I, primary distillation condensation II, primary distillation first-stage oil-water separation I and primary distillation oil-water separation II. Wherein the temperature of the cooling water in the primary distillation condensation I is 20 ℃, and the temperature of the cooling water in the primary distillation secondary condensation II is 30 ℃. Meanwhile, the temperature of the primary distillation liquid is controlled to be 40 ℃ by adjusting the flow of the first water vapor, the flow rate of the condensed water in the primary distillation condensation I and the flow rate of the condensed water in the primary distillation condensation II;
a redistillation stage: after the primary distillation liquid storage tank collects the primary distillation liquid, introducing 0.08MPa of second steam into the primary distillation liquid storage tank for distillation to obtain redistilled steam after distillation; redistilling the steam to obtain saturated aromatic water and volatile oil respectively after redistilling and condensing I, redistilling and condensing II and redistilling the oil-water separation; wherein the temperature of the cooling water in the redistillation condensate I is 10 ℃, and the temperature of the cooling water in the redistillation secondary condensate II is 30 ℃. Meanwhile, the temperature of the saturated aromatic water is controlled to be 30 ℃ by adjusting the flow of the second water vapor, the flow rate of the condensed water in the redistillation primary condensation I and the flow rate of the condensed water in the redistillation secondary condensation II.
The volatile oil prepared in example 1 was a clear, light yellow, transparent liquid. As can be seen, the volatile oil obtained in example 1 was hardly decomposed.
16 batches of the houttuynia cordata redistillate prepared in the example 1 are selected, and the batches are K100901-K100916. Then taking a proper amount of methyl n-nonanone reference substance, precisely weighing, and adding n-hexane to prepare a solution of 2 mg/ml. And then selecting the fingerprint and calibrating the characteristic peak. Methyl-n-nonanone is the main component in the houttuynia cordata double distillate, and the area percentage of the methyl-n-nonanone can be seen from the spectrogram, so that the methyl-n-nonanone is selected as an internal reference peak.
The internal reference peak methyl-n-nonanone is marked by S, and other common peaks are respectively marked by 1-10 in sequence. 7 common peaks are identified, which are respectively beta-pinene of peak 1, myrcene of peak 2, limonene of peak 3, 4-terpene alcohol of peak 7, d-terpineol of peak 8, borneol acetate of peak 9 and methyl n-nonanone of peak internal reference.
Establishing a common mode according to GC fingerprints of 16 batches of the houttuynia cordata redistillate, calculating the similarity of each batch by using the common mode as reference through traditional Chinese medicine fingerprint similarity calculation software, and obtaining the similarity evaluation result shown in the following table and figure 3.
| Batches of | Degree of similarity | Batches of | Degree of similarity |
| K100911 | 0.943 | K100901 | 0.994 |
| K100912 | 0.962 | K100902 | 0.997 |
| K100913 | 0.943 | K100903 | 0.989 |
| K100914 | 0.969 | K100904 | 0.976 |
| K100915 | 0.929 | K100905 | 0.987 |
| K100916 | 0.926 | K100906 | 0.997 |
| K100907 | 0.986 | ||
| K100908 | 0.995 | ||
| K100909 | 0.991 | ||
| K100910 | 0.987 |
As can be seen from the above table and FIG. 3, the relative retention time and the relative peak area of each fingerprint peak of 16 batches of saturated aromatic water with methyl-n-nonanone as the internal reference peak have better reproducibility. Thus, the houttuynia saturated aromatic water prepared in example 1 has very high quality batch-to-batch stability.
Preparing 16 batches of the saturated aromatic water of houttuynia cordata into injection, and measuring the content of the effective components according to Chinese pharmacopoeia to obtain the content of 4 components. The results of the content determination are shown in the following table.
The units in the following table are μ g/ml.
| Batches of | 4-terpene alcohols | Alpha-terpineol | Borneol acetate | Methyl n-nonanone |
| K100901 | 19.74 | 7.47 | 1.79 | 14.25 |
| K100902 | 17.36 | 6.14 | 1.63 | 12.22 |
| K100903 | 20.19 | 4.95 | 1.24 | 8.37 |
| K100904 | 26.94 | 5.26 | 1.48 | 8.93 |
| K100905 | 24.39 | 4.80 | 1.56 | 10.05 |
| K100906 | 15.11 | 5.15 | 1.28 | 8.68 |
| K100907 | 22.28 | 7.36 | 1.57 | 10.43 |
| K100908 | 19.30 | 6.96 | 1.53 | 10.35 |
| K100909 | 25.48 | 5.75 | 1.40 | 9.72 |
| K100910 | 25.54 | 5.21 | 1.51 | 10.71 |
| K100911 | 5.65 | 3.81 | 1.35 | 8.02 |
| K100912 | 11.43 | 4.94 | 2.06 | 12.94 |
| K100913 | 9.21 | 4.51 | 1.52 | 9.58 |
| K100914 | 6.49 | 2.84 | 1.39 | 7.92 |
| K100915 | 8.02 | 3.37 | 1.92 | 9.88 |
| K100916 | 6.33 | 3.81 | 1.95 | 12.87 |
Therefore, after the houttuynia saturated aromatic water prepared in the embodiment 1 is prepared into the injection, the content of the effective ingredients of the injection meets the standard of Chinese pharmacopoeia, and the product quality is high.
In addition, ten batches of the saturated aromatic water samples obtained in the example 1 are tested according to the quality standard of the houttuynia cordata re-distillate in Chinese pharmacopoeia, and the results are shown in the following table.
As can be seen from the above table, the property, pH value and bacterial endotoxin of the houttuynia saturated aromatic water prepared in example 1 all meet the standards of Chinese pharmacopoeia.
Comparative example 1
The difference from example 1 is that the preliminary distillation has only the preliminary distillation condensate I and no preliminary distillation condensate II.
As shown in fig. 5, the transparency of the volatile oil prepared in comparative example 1 was reduced, and it was seen that the volatile oil was partially decomposed.
Comparative example 2
The difference from example 1 is that the redistillation is only redistillation condensate I and not redistillation condensate II.
As shown in FIG. 6, the volatile oil prepared in comparative example 2 was very cloudy and it was seen that the volatile oil had decomposed.
Fingerprint detection
A batch of the saturated aromatic water prepared in example 1, comparative example 1 and comparative example 2 is taken, and fingerprint detection is carried out according to the fingerprint item of example 1. The method comprises the following specific steps: respectively and precisely absorbing 1ul of the reference substance solution and the test solution of the saturated aromatic water prepared in the example 1, the comparative example 1 and the comparative example 2, respectively injecting the test solution and the test solution into a gas chromatograph, cutting off the solvent peak 6 minutes before, recording a chromatogram, and calculating the similarity by using a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, wherein the similarity between the fingerprint of the test solution and the reference fingerprint is not lower than 0.9.
The results are shown in the following table and figure 4:
| item | Example 1 | Comparative example 1 | Comparative example 2 |
| Similarity of fingerprint | 1.000 | 0.808 | 0.720 |
As can be seen from the above table and fig. 4: the similarity of the finger prints of the saturated aromatic water prepared in the comparative example 1 and the saturated aromatic water prepared in the comparative example 2 is less than 0.9, and the finger prints do not meet the standard of Chinese pharmacopoeia. The degree of similarity of the saturated aromatic water prepared in example 1 was high. This indicates that the saturated aromatic water prepared in example 1 meets pharmacopoeia standards.
Comparative example 3
Comparative example 3 differs from example 1 in that the preliminary distillation only has preliminary distilled oil-water separation I and no preliminary distilled oil-water separation II.
As shown in fig. 7, the saturated aromatic water prepared in comparative example 3 contained oily substances, and thus it can be seen that the separation of the saturated aromatic water from the volatile oil was poor compared to the primary oil-water separation.
Example 2
A primary distillation stage: putting the houttuynia cordata into a multifunctional extraction tank, introducing first water vapor with the pressure of 0.04MPa, and distilling to obtain primary distillation vapor; and (3) respectively obtaining primary distillation liquid and volatile oil from the primary distillation steam after primary distillation condensation I, primary distillation condensation II, primary distillation first-stage oil-water separation I and primary distillation oil-water separation II. Wherein the temperature of the cooling water in the primary distillation condensation I is 5 ℃, and the temperature of the cooling water in the primary distillation secondary condensation II is 20 ℃. Meanwhile, the temperature of the primary distillation liquid is controlled to be 5 ℃ by adjusting the flow of the first water vapor, the flow rate of the condensed water in the primary distillation condensation I and the flow rate of the condensed water in the primary distillation condensation II;
a redistillation stage: after the primary distillation liquid storage tank collects the primary distillation liquid, introducing 0.04MPa of second steam into the primary distillation liquid storage tank for distillation to obtain redistilled steam after distillation; redistilling the steam to obtain saturated aromatic water and volatile oil respectively after redistilling and condensing I, redistilling and condensing II and redistilling the oil-water separation; wherein the temperature of the cooling water in the redistillation condensate I is 2 ℃, and the temperature of the cooling water in the redistillation secondary condensate II is 20 ℃. Meanwhile, the temperature of the saturated aromatic water is controlled to be 3 ℃ by adjusting the flow of the second water vapor, the flow rate of the condensed water in the redistillation primary condensation I and the flow rate of the condensed water in the redistillation secondary condensation II.
The volatile oil prepared in example 2 was a clear, light yellow, transparent liquid. As can be seen, the volatile oil obtained in example 1 was hardly decomposed. Meanwhile, 10 batches of the injection prepared from the saturated aromatic water prepared in example 2 were used for the measurement of the active ingredients, and the results are shown in the following table. The following table shows that the saturated aromatic water prepared in example 2 has high quality and meets the standards of Chinese pharmacopoeia.
The content of the houttuynia cordata injection is determined (unit: mug. ml)-1)
| Batches of | 4-terpene alcohols | Alpha-terpineol | Borneol acetate | Methyl n-nonanone |
| C100901 | 19.81 | 7.33 | 1.68 | 13.27 |
| C100902 | 22.66 | 8.07 | 1.82 | 14.06 |
| C100903 | 20.59 | 6.81 | 1.07 | 11.68 |
| C100904 | 32.17 | 6.23 | 1.79 | 11.33 |
| C100905 | 26.61 | 5.45 | 1.60 | 10.91 |
| C100906 | 20.90 | 7.68 | 1.40 | 9.67 |
| C100907 | 22.31 | 7.50 | 1.45 | 10.60 |
| C100908 | 24.44 | 9.43 | 1.83 | 14.98 |
| C100909 | 27.19 | 6.23 | 1.71 | 14.05 |
| C100910 | 28.29 | 5.71 | 1.74 | 12.81 |
Comparative example 4
Comparative example 4 differs from example 2 in that: in the primary distillation, the temperature of the primary distillation liquid is controlled to be 45 ℃ by adjusting the pressure of the first water vapor, the temperature of the condensed water in the primary distillation condensation I and the temperature of the condensed water in the primary distillation condensation II.
The volatile oil prepared in comparative example 4 was significantly less transparent and cloudy, and it can be seen that the preliminary distillation temperature exceeding 40 ℃ resulted in decomposition of the volatile oil.
Comparative example 5
Comparative example 5 differs from example 2 in that: in the redistillation, the temperature of the saturated aromatic water is controlled to be 35 ℃ by adjusting the pressure of the second water vapor, the temperature of the condensed water in the redistillation condensation I and the temperature of the condensed water in the redistillation condensation II.
The volatile oil prepared in comparative example 5 was remarkably reduced in transparency and was turbid, and thus it was seen that the temperature of saturated aromatic water exceeding 30 ℃ resulted in decomposition of the volatile oil.
Claims (9)
1. A method for extracting and separating volatile oil and saturated aromatic water from houttuynia cordata is characterized in that: the method comprises the following steps:
a primary distillation stage: distilling the houttuynia cordata by first steam to obtain primary distilled steam; performing primary distillation condensation I, primary distillation condensation II, primary distillation oil-water separation I and primary distillation oil-water separation II on the primary distillation steam to respectively obtain primary distillation liquid and volatile oil;
a redistillation stage: distilling the primary distilled liquid obtained by the primary distillation with second steam to obtain redistilled steam; carrying out redistillation condensation I, redistillation condensation II and redistillation oil-water separation on the redistilled steam to respectively obtain saturated aromatic water and volatile oil;
wherein in the primary distillation, the temperature of the primary distillation liquid is controlled to be not more than 40 ℃ and more than the freezing point of the primary distillation liquid; and in the redistillation, controlling the temperature of the saturated aromatic water to be not more than 30 ℃ and to be more than the freezing point of the saturated aromatic water.
2. The method of claim 1, wherein the extraction of volatile oil and aromatic water from houttuynia cordata comprises: in the primary distillation stage, the temperature of the primary distillation liquid is controlled by adjusting the pressure of the first steam, the temperature of the condensed water in the primary distillation condensate I and the temperature of the condensed water in the primary distillation condensate II.
3. The method of claim 2, wherein the extraction of volatile oil and aromatic water from houttuynia cordata comprises: the pressure of the first steam is 0.04-0.1 MPa; preferably, the pressure of the first steam is 0.04-0.08 MPa.
4. The method of claim 2, wherein the extraction of volatile oil and aromatic water from houttuynia cordata comprises: the temperature of cooling water in the primary distillation condensation I is 5-20 ℃; preferably, the temperature of the cooling water in the preliminary distillation condensation I is 6-18 ℃.
5. The method of claim 2, wherein the extraction of volatile oil and aromatic water from houttuynia cordata comprises: the temperature of cooling water in the primary distillation condensation II is 20-30 ℃; preferably, the temperature of the cooling water in the preliminary distillation condensation II is 22-28 ℃.
6. The method of claim 1, wherein the extraction of volatile oil and aromatic water from houttuynia cordata comprises: and regulating and controlling the temperature of the saturated aromatic water by regulating the pressure of the second water vapor, the temperature of the condensed water in the redistillation condensation I and the temperature of the condensed water in the redistillation condensation II.
7. The method of claim 6, wherein the volatile oil and aromatic water are extracted from houttuynia cordata, the method comprising: the pressure of the second steam is 0.04-0.1 MPa; preferably, the pressure of the second steam is 0.04-0.08 MPa.
8. The method of claim 6, wherein the volatile oil and aromatic water are extracted from houttuynia cordata, the method comprising: the temperature of cooling water in the redistillation condensation I is 0-10 ℃; preferably, the temperature of the cooling water in the redistillation condensate I is 0 to 8 ℃.
9. The method of claim 6, wherein the volatile oil and aromatic water are extracted from houttuynia cordata, the method comprising: the temperature of cooling water in the redistillation condensation II is 20-30 ℃; preferably, the temperature of the cooling water in the redistillation condensate II is 22 to 28 ℃.
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