Process for extracting pine needle volatile oil through ball-milling treatment and steam distillation

Abstract

The invention relates to the technical field of volatile oil extraction, in particular to a process for extracting pine needle volatile oil through ball-milling treatment and steam distillation, which comprises the following steps: (1) putting complete pine needle leaves into a ball mill for ball milling; (2) putting the pine needles subjected to ball milling in the step (1) into a container; (3) heating the container in a heating jacket, and carrying out steam distillation extraction; and (4) collecting volatile oil components at the upper half part of the light oil extractor after the extraction is completed, and adding anhydrous sodium sulfate to remove residual water. According to the process for extracting the pine needle volatile oil through ball milling treatment and steam distillation, cell walls of pine needles are damaged through ball milling, the dissolution rate of the volatile oil in cells of the pine needles is increased, the extraction rate of the volatile oil is increased, and simple and efficient extraction of the pine needle volatile oil is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of volatile oil extraction, and in particular to a process for extracting pine needle volatile oil by ball milling treatment and steam distillation. Background Art

[0002] Pine trees belong to the gymnosperms of the Pinaceae family and are widely distributed throughout my country, especially in the three northeastern provinces where the stock is relatively abundant. Pine needles grow rapidly, are harvested seasonally every year, and have a wide range of uses. Pine needles can be regarded as a natural plant resource that can be used sustainably. The volatile oil extracted from pine needles is a water-soluble compound with an aromatic odor and high volatility, which contains a wealth of active ingredients. Terpene components such as α-pinene and β-pinene have antitussive and expectorant effects, while sterols have antioxidant effects and prevent arteriosclerosis and hyperlipidemia. In addition, the vitamins and flavonoids in it also show strong antioxidant and antibacterial activities.

[0003] my country has a long history of using pine needles in the field of medical care. As early as in the "Famous Doctors' Records", it was recorded that "pine leaves are bitter and warm in taste, and are mainly used to treat rheumatism, promote hair growth, soothe the five internal organs, protect the middle, prevent hunger, and prolong life". "Compendium of Materia Medica" records that "pine needles are bitter, warm and non-toxic. Long-term use can prevent aging, lighten the body and invigorate the qi. They are mainly used to treat rheumatism, promote hair growth, soothe the five internal organs, protect the middle, prevent hunger, and prolong life". In modern times, pine needles have been widely studied and found to have broad application prospects in food, medicinal materials, chemical raw materials, health products and cosmetics.

[0004] The main extraction methods of pine needle essential oil include steam distillation, composite solvent extraction, supercritical CO2 extraction, microwave distillation, etc. Steam distillation has become the mainstream method for domestic and foreign manufacturers to extract essential oils due to its simple equipment, low cost and simple operation. However, the steam distillation method has the disadvantages of long extraction time and low extraction efficiency. This defect is because most of the volatile substances in pine needles exist in plant cells, and plant cells have cell walls. The intact cell walls will hinder the dissolution of volatile substances in the cells. Therefore, finding a way to destroy the plant cell wall can effectively increase the escape of essential oils, thereby improving the extraction efficiency and reducing the extraction time. Summary of the invention

[0005] The purpose of the present invention is to provide a process for extracting pine needle volatile oil by ball milling and steam distillation, wherein the cell walls of pine needles are destroyed by ball milling, and then the pine needle volatile oil is extracted by steam distillation, thereby achieving simple and efficient extraction of pine needle volatile oil and solving the problems existing in the above-mentioned background technology.

[0006] To achieve the above objectives, this application is implemented through the following technical solutions:

[0007] A process for extracting pine needle volatile oil by ball milling and steam distillation, comprising the following steps:

[0008] S1. Put fresh pine needles into a ball mill and grind them;

[0009] S2, placing the pine needles ball-milled in step S1 into a container;

[0010] S3, placing the container in a heating jacket for heating and performing steam distillation extraction;

[0011] S4. After the extraction is completed, the volatile oil components in the upper part of the light oil extractor are collected, and anhydrous sodium sulfate is added to remove the residual moisture.

[0012] Furthermore, in step S1, the ball milling speed is 240 r / min-400 r / min.

[0013] Furthermore, in step S1, the ball milling speed is 400 r / min.

[0014] Furthermore, in step S1, the ball milling time is 30 min-180 min.

[0015] Furthermore, in step S1, the ball milling time is 120 min.

[0016] Furthermore, the ball milling in step S1 is performed in two stages, wherein the ball milling speed in the first stage is lower than the ball milling speed in the second stage, and a set time is separated from the first stage.

[0017] Furthermore, the ball milling speed in the first stage is 240r / min-300r / min, and the ball milling speed in the second stage is 350r / min-400r / min.

[0018] Furthermore, the interval between the first stage and the second stage is 10-30 minutes.

[0019] Furthermore, the ball milling time of the first stage is 30-60 min, and the ball milling time of the second stage is 100-180 min.

[0020] The beneficial effects of the present invention are:

[0021] The present invention utilizes the pretreatment method of ball-milling pine needles to help break cell walls and improve extraction efficiency. The extracted pine needle volatile oil is analyzed and identified to have multiple chemical components and rich components through GC-MS analysis.

[0022] The ball milling process of the present invention is carried out in stages, and a set time interval is set between the two stages. The low-speed ball milling in the first stage is used to preliminarily destroy the cell wall of the pine needles. After the first stage of ball milling, the ball milling is stopped for a certain period of time to cool the pine needles in the ball mill, thereby preventing some substances from volatilizing or reacting with other components due to the increase in ball milling temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is the GC-MS total ion current diagram of pine needle essential oil in Example 1 of the present invention;

[0024] Figure 2 The effect of ball milling speed on the extraction rate in Examples 1-5 of the present invention;

[0025] Figure 3 This is the effect of ball milling time on the extraction rate in Examples 5-9 of the present invention. DETAILED DESCRIPTION

[0026] The technical solution of the present invention is described in detail below through examples. The following examples are merely exemplary and can only be used to explain and illustrate the technical solution of the present invention, but cannot be construed as limiting the technical solution of the present invention.

[0027] Example 1

[0028] The pine needles after ball milling were subjected to steam distillation. The ball mill speed was 80r / min, and the ball milling time was 120min. The volatile oil extraction rate was calculated to be 5mL / kg.

[0029] The obtained pine needle volatile oil was subjected to GC-MS detection, and the gas chromatography conditions were as follows: capillary quartz column (0.25mm×0.25μm, length 30m), the vaporization chamber and injection temperature were set to 230℃ and 280℃ respectively; the temperature program was: first maintained at 60℃ for 5min, then increased from 60℃ to 120℃ at a rate of 10℃ / min and maintained for 5min, then increased from 120℃ to 200℃ at the same rate and maintained for 5min, and then increased from 200℃ to 280℃ at the same rate and maintained for 15min; the carrier gas was high-purity helium with a flow rate of 1.0mL / min; the injection volume was 1μL; the split ratio was 1:20.

[0030] Mass spectrometry conditions: electron impact (EI) ion source; electron energy of 70 eV; scanning range of 15-500 amu.

[0031] The chemical components and relative mass fractions of pine needle essential oil are shown in Table 1. Figure 1 shown.

[0032] Table 1

[0033]

[0034] Table 1

[0035]

[0036] Table 1

[0037]

[0038] Example 2

[0039] The similarities between this embodiment and embodiment 1 are not repeated here, except that the ball mill speed is 160 r / min, the ball milling time is 120 min, and the volatile oil extraction rate is 5.3 mL / kg.

[0040] Example 3

[0041] The similarities between this embodiment and embodiment 1 are not repeated here, except that the ball mill speed is 240 r / min, the ball milling time is 120 min, and the volatile oil extraction rate is 5.5 mL / kg.

[0042] Example 4

[0043] The similarities between this embodiment and embodiment 1 are not repeated here, except that the ball mill speed is 320 r / min, the ball milling time is 120 min, and the volatile oil extraction rate is 5.9 mL / kg.

[0044] Example 5

[0045] The similarities between this embodiment and embodiment 1 are not repeated here, except that the ball mill speed is 400 r / min, the ball milling time is 120 min, and the volatile oil extraction rate is 6 mL / kg.

[0046] Example 6

[0047] The similarities between this embodiment and embodiment 1 are not repeated here, except that the ball mill speed is 400 r / min, the ball milling time is 30 min, and the volatile oil extraction rate is 4.7 mL / kg.

[0048] Example 7

[0049] The similarities between this embodiment and embodiment 1 are not repeated here, except that the ball mill speed is 400 r / min, the ball milling time is 60 min, and the volatile oil extraction rate is 5.5 mL / kg.

[0050] Example 8

[0051] The ball mill was used at a rotation speed of 80 r / min for 30 min, then the ball milling was stopped for 20 min, and then the ball milling was performed at a rotation speed of 400 r / min for 100 min. Then, steam distillation was performed, and the volatile oil extraction rate was 6.2 mL / kg.

[0052] Example 9

[0053] The similarities between this embodiment and embodiment 8 are not repeated here. The difference is that in the first stage, the ball mill speed is 120 r / min, the ball milling time is 60 min, and the ball milling is stopped for 30 min. In the second stage, the ball mill speed is 380 r / min for 120 min, and then steam distillation is performed. The volatile oil extraction rate is 6.1 mL / kg.

[0054] Comparative Example 1

[0055] The similarities between this comparative example and Example 1 are not repeated here, except that the pine needles were not subjected to ball milling. The volatile oil extraction rate was 5 mL / kg.

[0056] It can be seen from Example 1 and Comparative Example 1 that after ball milling, the yield of volatile oil is higher and the efficiency is higher. By comparing Examples 8 and 9 with other Examples, the yield of volatile oil is higher.

[0057] Therefore, the present invention adopts the above-mentioned ball milling treatment and steam distillation process for extracting pine needle volatile oil, destroys the pine needle cell wall by ball milling, and then uses steam distillation for extraction, thereby achieving simple and efficient extraction of pine needle volatile oil.

[0058] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solution of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solution to deviate from the spirit and scope of the technical solution of the present invention.

Claims

1. A process for extracting pine needle volatile oil by ball milling and steam distillation, characterized in that: Use the following steps: S1. Put fresh pine needles into a ball mill and grind them; S2, placing the pine needles ball-milled in step S1 into a container; S3, placing the container in a heating jacket for heating and performing steam distillation extraction; S4. After the extraction is completed, the volatile oil components in the upper part of the light oil extractor are collected, and anhydrous sodium sulfate is added to remove the residual moisture.

2. The process for extracting pine needle essential oil by ball milling steam distillation according to claim 1, characterized in that: In step S1, the ball milling speed is 240r / min-400r / min.

3. The process for extracting pine needle essential oil by ball milling steam distillation according to claim 2, characterized in that: In step S1, the ball milling speed is 400 r / min.

4. The process for extracting pine needle essential oil by ball milling steam distillation according to claim 1, characterized in that: In step S1, the ball milling time is 30 min-180 min.

5. The process for extracting pine needle essential oil by ball milling steam distillation according to claim 4, characterized in that: In step S1, the ball milling time is 120 min.

6. The process for extracting pine needle essential oil by ball milling steam distillation according to claim 1, characterized in that: The ball milling in step S1 is carried out in two stages, wherein the ball milling speed in the first stage is lower than the ball milling speed in the second stage, and there is a set time interval between the first stage and the second stage, and the ball milling time in the second stage is longer than the ball milling time in the first stage.

7. The process for extracting pine needle essential oil by ball milling and steam distillation according to claim 6, characterized in that: The ball milling speed in the first stage is 240r / min-300r / min, and the ball milling speed in the second stage is 350r / min-400r / min.

8. The process for extracting pine needle essential oil by ball milling and steam distillation according to claim 6, characterized in that: The interval between the first and second stages is 10-30 minutes.

9. The process for extracting pine needle essential oil by ball milling and steam distillation according to claim 6, characterized in that: The ball milling time of the first stage is 30-60min, and the ball milling time of the second stage is 100-180min.

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