CN104774692A - Extraction method of black pepper volatile oil - Google Patents

Abstract

The invention relates to a method for extracting black pepper volatile oil. The method comprises: crushing freshly picked black pepper, air-dried, cold-stored, and dried black pepper, extracting for several hours by steam distillation-ether extraction, salting out, and drying The solvent is dried, the solvent is recovered under reduced pressure, and the product is obtained. It makes the operation easier, the extraction time is shorter, and at the same time avoids the influence of the traditional steam distillation method on the extraction rate due to the adsorption of some essential oils on the wall of the extractor. It is currently widely used in the extraction of volatile components such as black pepper. It is a kind of black pepper New technology for volatile oil extraction.

Description

A kind of extraction method of black pepper volatile oil

technical field

The invention relates to a method for extracting black pepper volatile oil.

Background technique

Volatile oil is also called essential oil, essential oil or aromatic oil. The composition of essential oil is mainly composed of terpenoids (mainly monoterpenes and sesquiterpenes), as well as non-terpenoid aromatics and aliphatics. Volatile oil (essential oil), as one of the effective components of pepper, has a variety of biological activities and physiological effects, and has shown gratifying effects on the cardiovascular and cerebrovascular systems, nervous system, and digestive system. Because it has a good inhibitory effect on a variety of bacteria and fungi, it can accelerate blood circulation in local tissues and promote epithelial cell regeneration, so it can play a role in detoxification, weight loss, beauty and moisturizing; in addition, it can be used in food processing industry, As a food preservative and flavoring agent, it can improve food aroma; at the same time, because it can stimulate gastrointestinal peristalsis, it can promote digestion and absorption. Pepper essential oil has no toxic and side effects, and can be processed into products with different uses.

The most commonly used extraction methods of pepper volatile oil are cold pressing, steam distillation, organic solvent leaching, ultrasonic-assisted extraction, microwave-assisted extraction, Soxhlet-assisted extraction, simultaneous distillation and extraction, supercritical fluid extraction, etc. . Yang Xiaoyan et al. (Southwest University for Nationalities, 2009, 35 (3): 556) extracted the volatile oil of white pepper by steam distillation, selected the volume of volatile oil as an index to design an orthogonal experiment, and optimized the extraction conditions; Zhao Lijuan et al. (Anshan Iron and Steel Institute, 2006, 17 (5): 848-850) extracted the volatile oil components of white pepper in Hainan area by distillation extraction method, and measured the mass fraction of white pepper volatile oil; Liu Xuewu et al. ) used a supercritical fluid extraction test device to investigate the optimal extraction process of pepper volatile oil; Zhang Guohong et al. (Food Industry, 1997,18(11):21-25) used ethanol as a solvent and used a uniform design to extract pepper components.

Because the essential oil content in plants is extremely small, and the obtained essential oil has complex components, it is difficult to purify. Solvent extraction of essential oils is a commonly used extraction method. Although the equipment is simple, cheap, and high in yield, it requires a large amount of organic solvents and contains many impurities; although supercritical _CO2 fluid extraction has high efficiency, low temperature, high yield, and green It has the advantages of chemicalization and no solvent residue, but the equipment investment is large, the process technology requirements are high, and the limitations are great.

Contents of the invention

The invention provides a method for extracting pepper essential oil by a simultaneous distillation extraction method, which is characterized in that steam distillation and distillate extraction with an organic solvent are combined into one step for extraction. It makes the operation easier, the extraction time is shorter, and at the same time avoids the influence of the traditional steam distillation method on the extraction rate due to the adsorption of some essential oils on the wall of the extractor. It is currently widely used in the extraction of volatile components such as black pepper. It is a kind of black pepper New technology for volatile oil extraction.

The extraction method of black pepper volatile oil of the present invention comprises the following contents:

Black pepper is a freshly picked fruit, first rinsed with distilled water, protected from light, and then stored in the refrigerator for later use;

The black pepper powder stored in the refrigerator is sieved to make medicinal powder with different meshes such as 120-180 mesh;

Weigh 50.00g of a certain mesh of black pepper, and the amount of solvent is 20 to 50 times;

Soak in 150 mL of distilled water and 100 mL of ether for 0~8 hours;

The extraction temperature is below 100℃, and the extraction time is 8~16h;

The extraction method is steam distillation;

The emulsion formed by salting out the volatile oil containing water was salted out with sodium chloride, extracted with 10 mL of ether, and dried over anhydrous sodium sulfate.

Put black pepper in a three-necked flask, soak it with a certain amount of distilled water for different periods of time, add distilled water according to a certain amount of solvent, add ether, and steam the steam generator to extract for several hours. Control the extraction temperature to prevent the raw material from being overheated. Heating and coking changes the composition. The extracted product was fully cooled, extracted several times with ether until the liquid was colorless, dried over anhydrous sodium sulfate, and the ether was collected by rotary evaporation to obtain black pepper volatile oil, a light yellow transparent liquid, with an extraction rate of up to 2.6572%. Various chemical constituents were identified in black pepper volatile oil by GC-MS.

The steam generator in the step refers to the instrument for extracting volatile oil.

In the step, GC-MS gas chromatography-mass spectrometry is used for analysis and identification, and the chemical components of the black pepper volatile oil are distilled and extracted. GC conditions: Chromatographic column: RTX-5MS quartz capillary column (30m×0.32mm×0.25μm), vaporization temperature: 290°C, heating program: keep at 60°C for 3min, then rise to 100°C at a rate of 3°C/min, Rise to 200°C at a rate of ℃/min, then rise to 290°C at a rate of 8°C/min and hold for 20 minutes, the carrier gas is helium (99.999%), the flow rate is 1.90ml/min, the pressure is 32.1kPa, and the diaphragm is purged at 3.0mL/min. The split ratio is 50:1, and the injection volume is 0.2 μL. MS conditions: electron energy 70 eV, transfer line temperature 250°C, ion source temperature 230°C, detection voltage 0.90kv, mass scanning range m/z: 33-600, recording 3~65min.

Extraction rate of volatile oil in the step=mass of volatile oil/sample quality×100%.

Nearly 30 chemical constituents were identified in the essential oil of black pepper by GC-MS in the step. The main ingredients are: carene, a-pinene, camphene, caryophyllene, copaene, wintergreen, beta-pinene, myrcene, caryophyllene oxide, phellandrene, ocimene, r-pine Oleene, naphthene, sabinene hydrate, limonene oxide, a-terpineol, heptadecane, etc. Among them, there are 17 kinds of alkenes, accounting for 86.8% of the total.

The present invention obtains technical progress:

1. The present invention extracts volatile oil from black pepper, adopts the combination of steam distillation and organic solvent extraction, not only makes the operation easier, the extraction time is short, but also avoids the influence of the traditional steam distillation method due to the adsorption of part of the essential oil on the wall of the extractor. Extraction rate of volatile oil;

2. In the "List of Dangerous Goods" (GB 12268-90) of the People's Republic of China, some organic solvents belong to the first class of dangerous goods controlled by precursors. This method can reduce the amount of ether used, avoid pollution to the environment, and improve safety sex;

3. The extraction device is simple and easy to operate, and the material consumption has obvious advantages compared with other methods, and the extraction rate of volatile oil has been significantly improved.

Detailed ways

Example 1:

Crush black pepper through a 120-mesh sieve, weigh 50.00g and place it in a 2000mL three-neck flask, soak it in 150mL distilled water for 6h, add 100mL ether, add distilled water to 8 times the amount of solvent, and extract with steam for 12h , control the extraction temperature below 100°C. The extracted product was fully cooled, extracted with 10 mL of ether each time until the liquid was colorless, dried with anhydrous sodium sulfate, and collected by rotary evaporation to obtain a light yellow transparent liquid, namely black pepper volatile oil, with an extraction rate of 2.5974%.

Example 2:

Crush black pepper through a 120-mesh sieve, weigh 50.00g and place it in a 2000 mL three-neck flask, soak it in 150 mL of distilled water for 8 hours, add 100 mL of diethyl ether, add distilled water to 9 times the amount of solvent, and extract with steam for 14 hours , control the extraction temperature below 100°C. The extracted product was fully cooled, extracted with 10 mL of ether each time until the liquid was colorless, dried with anhydrous sodium sulfate, and collected by rotary evaporation to obtain a light yellow transparent liquid, namely black pepper volatile oil, with an extraction rate of 2.6087%.

Example 3:

Crush black pepper through a 140-mesh sieve, weigh 50.00 g and place it in a 2000 mL three-necked flask, soak it in 150 mL distilled water for 4 hours, add 100 mL of ether, add distilled water to 8 times the amount of solvent, and extract with steam for 14 hours , control the extraction temperature below 100°C. The extracted product was fully cooled, extracted with 10 mL of ether each time until the liquid was colorless, dried with anhydrous sodium sulfate, and collected by rotary evaporation to obtain a light yellow transparent liquid, namely black pepper volatile oil, with an extraction rate of 2.6481%.

Example 4:

Crush black pepper through a 160-mesh sieve, weigh 50.00 g and place it in a 2000 mL three-neck flask, soak it in 150 mL distilled water for 8 hours, add 100 mL of ether, add distilled water to 8 times the amount of solvent, and inject water vapor into the steam generator to extract for 8 hours , control the extraction temperature below 100°C. The extracted product was fully cooled, extracted with 10 mL of ether each time until the liquid was colorless, dried with anhydrous sodium sulfate, and collected by rotary evaporation to obtain a light yellow transparent liquid, namely black pepper volatile oil, with an extraction rate of 2.4859%.

Claims (5)

1. Black pepper is a freshly picked fruit, first rinsed with distilled water, protected from light, and then stored in the refrigerator for later use; The black pepper powder stored in the refrigerator is sieved to make medicinal powder with different meshes such as 120-180 mesh; Weigh 50.00g of a certain mesh of black pepper, and the amount of solvent is 20 to 50 times; Soak in 150 mL of distilled water and 100 mL of ether for 0~8 hours; The extraction temperature is below 100℃, and the extraction time is 8~16h; The extraction method is steam generator distillation; The emulsion formed by salting out the volatile oil containing water was salted out with sodium chloride, extracted with 10 mL of ether, and dried over anhydrous sodium sulfate. 2. Put black pepper in a three-necked flask, soak it with a certain amount of distilled water for different times, add distilled water according to a certain amount of solvent, add ether, and steam the steam generator to extract for several hours, control the extraction temperature to prevent the raw material from being too high Coking by strong heating causes the composition to change; The extracted product was fully cooled, extracted several times with ether until the liquid was colorless, dried over anhydrous sodium sulfate, and the ether was collected by rotary evaporation to obtain black pepper volatile oil, a light yellow transparent liquid, with an extraction rate of up to 2.6572%. 3. A variety of chemical components were identified in the volatile oil of black pepper by GC-MS, In the step, GC-MS gas chromatography-mass spectrometry is used for analysis and identification, and the chemical components of black pepper volatile oil are distilled and extracted. GC conditions: chromatographic column: RTX-5MS quartz capillary column (30m × 0.32mm × 0.25μm), vaporization temperature: 290 ℃, heating program: keep at 60°C for 3 minutes, then rise to 100°C at a rate of 3°C/min, rise to 200°C at a rate of 5°C/min, rise to 290°C at a rate of 8°C/min and hold for 20 minutes, the carrier gas is helium Gas (99.999%), flow rate 1.90ml/min, pressure 32.1kPa, diaphragm purge 3.0mL/min, split ratio 50:1, injection volume 0.2μL; MS conditions: electron energy 70 eV, transfer line temperature 250°C, ion source temperature 230°C, detection voltage 0.90kv, mass scanning range m/z: 33-600, recording 3~65min. 4. Nearly 30 chemical components were identified in the GC-MS black pepper volatile oil in the step, The main ingredients are: carene, a-pinene, camphene, caryophyllene, copaene, wintergreen, beta-pinene, myrcene, caryophyllene oxide, phellandrene, ocimene, r-pine There are 17 kinds of olefinic compounds such as oleene, naphthene, hydrated sabinene, limonene oxide, a-terpineol, and heptadecane, accounting for 86.8% of the total. The extraction rate of volatile oil in the step = volatile oil mass/sample mass×100% . 5. The present invention has made technological progress: 1. The present invention extracts volatile oil from black pepper, adopts the combination of steam distillation and organic solvent extraction, not only makes the operation easier, the extraction time is short, but also avoids the influence of the traditional steam distillation method due to the adsorption of part of the essential oil on the wall of the extractor. Extraction rate of volatile oil; 2. In the "List of Dangerous Goods" (GB 12268-90) of the People's Republic of China, some organic solvents belong to the first class of dangerous goods controlled by precursors. This method can reduce the amount of ether used, avoid pollution to the environment, and improve safety sex; 3. The extraction device is simple and easy to operate, and the material consumption has obvious advantages compared with other methods, and the extraction rate of volatile oil is significantly improved.