CN113521220A

CN113521220A - Preparation method of galangal cell water and application of galangal cell water

Info

Publication number: CN113521220A
Application number: CN202010291079.3A
Authority: CN
Inventors: 屈恋; 何健; 容宝珊; 郑晓旻; 艾勇; 何廷刚
Original assignee: Guangdong Heji Biotechnology Co ltd
Current assignee: Guangdong Heji Biotechnology Co ltd
Priority date: 2020-04-14
Filing date: 2020-04-14
Publication date: 2021-10-22

Abstract

The invention discloses a preparation method of galangal cell water, which can obtain pure natural galangal cell water at a lower temperature (30-65 ℃) without adding any solvent through the organic combination of a low-temperature vacuum (reduced pressure) extraction technology and an enzymolysis technology. The galangal cell water obtained by the method disclosed by the invention is high in quality, contains more than 70 volatile active ingredients, is aromatic and soft in smell, is high in safety to a human body, and has a certain moisturizing effect; can be used as green natural raw material in the fields of food, health product, medicine and cosmetic.

Description

Preparation method of galangal cell water and application of galangal cell water

Technical Field

The invention relates to the technical field of agricultural product treatment, in particular to a preparation method of galangal cell water and application of the obtained galangal cell water.

Background

Alpinia officinarum Hance (Alpinia officinarum Hance) is also called lesser galangal rhizome or lesser galangal rhizome. Perennial herbs with cylindrical roots and stems are warm in nature, pungent in flavor and fragrant in flavor; there are joints, which have the scale of the ring membrane material and root on the joints. Is distributed in Yunnan, Guangdong, Guangxi and Taiwan. Rhizoma Alpiniae Officinarum has effects of dispelling pungent and warm, dredging collaterals, dispelling cold, and relieving pain, and can be used for treating abdominal psychroalgia, stomach cold emesis, belch and acid regurgitation. The galangal is rich in volatile oil and flavonoid components, and the main components of the volatile oil comprise 1, 8-cineole, methyl cinnamate, eugenol, pinene, piper cubebene, pungent galangal components and the like; the flavone components mainly comprise galangin, kaempferide, kaempferol, quercetin, isorhamnetin, etc. The application of galangal is greatly limited because of its strong pungent taste.

The conventional method for extracting galangal is a solvent extraction method, which mainly aims at extracting a certain target component. After the extraction, a series of subsequent purification treatments (such as solvent removal by reduced pressure distillation) are required, the solvent cannot be completely removed by reduced pressure distillation, and the residual organic solvent brings certain hidden dangers to the health of users. Chinese patent application CN108740636A discloses a process for extracting ginger juice, which comprises directly pulping ginger, extracting with water at low temperature, and filtering to obtain ginger juice. The method cannot sufficiently extract aromatic active substances, has insufficient fragrance, and the obtained extractive solution has strong pungency and contains a large amount of plant tissues (with granular feeling).

For the extraction of plants, the chinese patent application CN109730948A discloses a method for preparing peony flower cell water by combining an ultrasonic low-temperature rotary steaming method and an enzyme method: firstly, squeezing to obtain juice and residue 1, then carrying out rotary evaporation on the residue 1 to obtain cell water 1 and residue 2, and finally carrying out enzymatic hydrolysis on the residue 2 and then carrying out rotary evaporation to obtain cell water 2. And mixing the juice, the cell water 1 and the cell water 2 to obtain the high-yield peony cell water. The method has high extraction efficiency, but has the following defects: (1) the squeezing method is adopted and then mixed with the liquid obtained by the vacuum extraction method, so that polysaccharide, pigment and pungent smell are brought in, and the problems of corrosion prevention and decoloration are caused; (2) the method solves the problem of corrosion resistance by being matched with other plants for distillation at the later stage of the process, but easily changes the original water content and smell of the peony cells, and the quality cannot be controlled in the later-stage production.

Disclosure of Invention

The invention aims to overcome the technical defects and provide a preparation method of galangal cell water, which is clear and transparent, fragrant and soft in smell and high in safety, and the galangal cell water is rich in various active ingredients.

The invention is realized by the following technical scheme:

a preparation method of galangal cell water comprises the following steps: adding no solvent, primarily extracting galangal at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, condensing galangal cell water to form steam, collecting liquid, extracting for 1.5-2.5 hours to obtain primary extracted cell water and primary extracted galangal residue, adding 0.2-0.4 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary galangal into the primary extracted cell water, then pouring the mixture into the primary extracted galangal residue, extracting again at the temperature of 30-45 ℃ and under the pressure of-80 kPa to-101 kPa, and collecting galangal cell water after 3-7 hours of extraction.

The galangal is cut into ginger slices with the thickness of 1 mm-10 mm and then extracted, so that the extraction speed is accelerated and the full extraction is facilitated.

The primary extraction time is one of key parameters, if the time is too short, the extracted galangal cell water is too little, and the cell water is difficult to wet galangal residues after enzyme is added, so that the enzymolysis cannot be normally carried out. If the primary extraction time is too long, cell water flows out too much, so that the subsequent extraction efficiency is reduced, the enzymolysis time is prolonged, and the risk of excessive enzymolysis is brought. According to the invention, a certain amount of enzyme is added into the primary cell extraction water, and the primary cell extraction water is put into the container again to extract the galangal residues, so that the method has the following beneficial advantages: firstly, the surface tension of primary extracted cell water is low, and the permeability is good; secondly, the pH of the primary cell extracting water is 3-7, and the pH does not need to be additionally adjusted, so that the enzyme activity is favorably improved; thirdly, the enzymolysis can accelerate the wall breaking; fourth, low temperature vacuum technique. Through the synergy of the four effects, the enzymolysis speed can be controlled at a lower temperature (30-45 ℃) to accelerate the cell sap outflow speed. The primary extraction cell water poured back into the container is steamed in about the first 1 hour in the secondary extraction step, the enzymolysis speed is high in the period, the enzymolysis time is controlled by the amount of the primary extraction liquid and the process conditions of secondary extraction (at the moment, the amount of the primary extraction liquid is important, the enzymolysis time is prolonged, the enzymolysis is excessive, the enzymolysis time is shortened, the enzymolysis is insufficient), and the problems that the cell liquid is diluted due to the addition of a large amount of water and the odor is stimulated due to the excessive enzymolysis in the traditional enzymolysis method are solved.

The permeability of the initially improved galangal cell water is better than that of pure water, and experiments show that about 80% more flavone and polysaccharide can be extracted by using the galangal cell water as a solvent than by using the pure water as the solvent when extracting the galangal residue by a solvent method.

Preferably, the temperature of the primary extraction stage is 35-50 ℃, and the pressure is-80 kPa-101 kPa. The preferred temperature and pressure are such that the cellular water can be well exuded and evaporated, while the activity of the volatilized cellular water can be retained at a lower temperature.

Preferably, the addition amount of the cellulase is 0.25-0.35%, and the addition amount of the pectinase is 0.01-0.06%. The enzyme is macromolecular protein, can be adsorbed on the surfaces of galangal residue cells within the addition range, is difficult to volatilize under low-temperature vacuum conditions, and does not need subsequent treatment.

Stirring is carried out in the extraction process, and the stirring speed is 1-150 revolutions per minute. The galangal is uniformly heated, local high temperature is prevented, and meanwhile, the extraction rate can be increased, so that the cell water can be fully extracted; and the galangal residues and the primary cell extraction water added with the enzyme can be uniformly mixed by stirring in the secondary extraction step, so that all the galangal residues are fully infiltrated, and the enzymolysis is ensured.

Condensing in the collecting process, wherein the condensing temperature is-10-8 ℃.

The pungent components of the galangal are extremely easy to volatilize, so that the galangal is difficult to collect in the low-temperature vacuum extraction process, the pungent sense of galangal cell water can be weakened to the very great extent, and the problem of limited application due to the pungent and pungent sense of the galangal is solved.

The galangal provided by the invention adopts galangal rhizome, and the active ingredient content of the galangal rhizome is high; preferably, the galangal is fresh galangal, which is full of water, free of mildew and rot, and not baked or dried in the sun. Generally, fresh galangal is not more than two weeks after being picked, and can also be stored for a long time by means of freshness preservation such as refrigeration.

The galangal cell water prepared by the method can be applied to the fields of food, health-care products, medicines, cosmetics and the like.

Compared with the prior art, the invention has the following beneficial effects:

the invention organically combines a low-temperature vacuum (reduced pressure) extraction technology with an enzymolysis technology, performs primary extraction on the galangal by the low-temperature vacuum (reduced pressure) extraction technology, and uses the high permeability of primary extracted cell sap as an enzymolysis solvent to perform secondary extraction on galangal residues. Compared with a single low-temperature vacuum extraction technology, the extraction rate of the cell sap is higher, and more active ingredients can be obtained; meanwhile, the problem that the traditional enzymolysis method is easy to carry out enzymolysis excessively so that the extracting solution has foreign flavor is solved.

The galangal cell water obtained by the method is clear and transparent and is light brown yellow; is rich in more than 70 volatile active ingredients; the galangal fruit mask has the advantages of soft and fragrant smell (the special fragrant smell of galangal is preserved, and the pungent and pungent feeling brought by galangal is avoided), high safety and certain moisturizing effect; can be applied to the fields of food, health products, medicines, cosmetics and the like.

Drawings

FIG. 1 is a histogram of the data of the galangal cell water safety test of example 1.

Detailed Description

The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.

The alpinia officinarum used in the examples and comparative examples was fresh rhizome of alpinia officinarum, hanjiang, Guangdong. Cleaning, draining, cutting into ginger slices with the thickness of 2-3 mm, and carrying out extraction experiments.

Example 1:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 35 ℃ and under the pressure of-101 kPa, forming galangal cell water into steam, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted galangal residues, adding 145g of cellulase and 25g of pectinase into the primary extracted cell water, then pouring into the primary extracted galangal residues, extracting again at 35 ℃ and under the pressure of-101 kPa, and finishing extraction for 6.5 hours; stirring at 45 r/min in the whole process, and condensing at-8 deg.C; 28.8kg of galangal cell water is collected, and the liquid is clear and transparent, light brown yellow, aromatic and soft in smell and free of spicy feeling.

Example 2:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 50 ℃ and under the pressure of-80 kPa, forming galangal cell water into steam, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted galangal residues, adding 125g of cellulase and 30g of pectinase into the primary extracted cell water, then pouring into the primary extracted galangal residues, extracting again at 45 ℃ and under the pressure of-90 kPa, and finishing extraction for 5 hours; stirring at 60 r/min in the whole process, and condensing at-8 deg.C; 28.1kg of galangal cell water is collected, and the liquid is clear and transparent, light brown yellow, aromatic and soft in smell and free of spicy feeling.

Example 3:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 65 ℃ and under the pressure of-60 kPa, forming galangal cell water into steam, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted galangal residues, adding 170g of cellulase and 10g of pectinase into the primary extracted cell water, then pouring into the primary extracted galangal residues, extracting again at 40 ℃ and under the pressure of-90 kPa, and finishing extraction for 6 hours; stirring at 80 r/min, and condensing at-8 deg.C; 28.5kg of galangal cell water is collected, and the liquid is clear and transparent, light brown yellow, aromatic and soft in smell and free of spicy feeling.

Example 4:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 40 ℃ and under the pressure of-101 kPa, forming galangal cell water into steam, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted galangal residues, adding 100g of cellulase and 45g of pectinase into the primary extracted cell water, then pouring into the primary extracted galangal residues, extracting again at 45 ℃ and under the pressure of-90 kPa, and finishing extraction for 4.5 hours; stirring at 60 r/min in the whole process, and condensing at-8 deg.C; 27.6kg of galangal cell water is collected, and the liquid is clear and transparent, light brown yellow, aromatic and soft in smell and free of spicy feeling.

Example 5:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 30 ℃ and under the pressure of-101 kPa, forming galangal cell water into steam, condensing and collecting liquid, extracting for 2.5 hours to obtain primary extracted cell water and primary extracted galangal residues, adding 200g of cellulase and 5g of pectinase into the primary extracted cell water, then pouring into the primary extracted galangal residues, extracting again at 30 ℃ and under the pressure of-101 kPa, and finishing extraction for 7 hours; stirring at 45 r/min in the whole process, and condensing at-8 deg.C; collecting 29.4kg of galangal cell water, wherein the liquid is clear and transparent, light brown yellow, aromatic and soft in smell and free of pungent taste.

Comparative example 1:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, extracting at 35 ℃ and-101 kPa, condensing cell water after the cell water forms steam, collecting liquid, extracting for 8.5 hours, stirring at 45 r/min in the whole process, and condensing at-8 ℃ to obtain 22.8kg of galangal cell water, wherein the liquid is clear and transparent, light brown yellow and light in fragrance.

Comparative example 2:

putting 50kg of galangal into 150L low-temperature extraction equipment, mixing with 5kg of water, 145g of cellulase and 25g of pectinase, stirring for 45 minutes at 35 ℃, extracting at 35 ℃, under-101 kPa, condensing galangal cell water to form steam, collecting liquid, stirring for 45 revolutions per minute in the whole process, extracting for 8.5 hours at the condensation temperature of-8 ℃, collecting 31.7kg of galangal cell water (containing 5kg of additionally added water), and obtaining clear and transparent liquid which is light brown yellow, light in fragrance and has foreign flavor.

Comparative example 3:

putting 50kg of galangal into 150L low-temperature extraction equipment, mixing with 5kg of water, 145g of cellulase and 25g of pectinase, extracting at 35 ℃ under normal pressure and stirring at 60 rpm for 8.5 hours, filtering (double filtration: filtering by a centrifugal machine and then filtering by a 0.22 mu m filter membrane) and collecting 33.5kg of galangal cell water (containing 5kg of additionally added water), wherein the liquid is dark brown, slightly turbid, light in fragrance and heavy in peculiar smell.

Comparative example 4:

putting 50kg of galangal into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 35 ℃ and under the pressure of-101 kPa, forming galangal cell water into steam, condensing and collecting liquid, extracting for 0.5 h to obtain primary extracted cell water and primary extracted galangal residue, adding 145g of cellulase and 25g of pectinase into the primary extracted cell water, pouring into the primary extracted galangal residue, extracting again at 35 ℃ and under the pressure of-101 kPa, and finishing extraction for 6.5 h; stirring at 45 r/min in the whole process, and condensing at-8 deg.C; collecting 26.2kg of rhizoma Alpiniae Officinarum cell water, and collecting clear and transparent liquid with light brown yellow color, light fragrance, and no pungency.

The test methods are as follows:

1. volatile active ingredient analysis of galangal cell water: the headspace gas quality was checked at 80 ℃ injection temperature.

(1) Instrument information: agilent 7980 AGC; MS 5975C; 50/30 μm CAR/PDMS/DVB extraction fiber head, SUPELCO USA.

(2) GC-MS conditions: the chromatographic column is HP-INNOWAX capillary column (30m × 0.25mm × 0.25 μm); the carrier gas is He, the flow rate is 1mL/min, and the separation ratio is 5: 1; the sample injection temperature is 250 ℃; the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 5min, the temperature is raised to 250 ℃ at the speed of 8 ℃/min, and the temperature is kept for 5 min.

Mass spectrum conditions: EI ionization source, energy 70 eV; the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, the interface temperature is 250 ℃, and the scanning range is 30-400 m/z.

(3) Sample pretreatment: 5mL of the sample and 1g of NaCl were placed in a 20mL headspace bottle, and the cap was screwed down. After 5min of equilibrium at 80 ℃ in stirring mode, extracting for 5min at 80 ℃ with a solid phase micro-extraction needle, and then resolving for 5min at the sample inlet.

Table 1: example 1 results of volatile active ingredient analysis of Alpinia galanga cells in Water (Low match and relative content of ingredients not listed)

(2) Galangal cell water safety test

The HaCaT cell is a human immortal epidermal cell line, has cytotoxicity to the HaCaT cell, and can be used as reference data for safety of skin. The normal cells are in vigorous metabolism, succinate dehydrogenase in mitochondria can reduce tetrazolium salt substances into colored crystalline substances and deposit the crystalline substances around the cells, OD values can be read by an enzyme labeling instrument according to the change, and the relative growth condition of the cells can be known by comparing the OD values with a blank control group. Example 1 the results of the galangal cell water safety test are shown in figure 1.

It is illustrated by figure 1 that galangal cell water is substantially non-toxic to human epidermal cells.

(3) Moisturizing efficacy test of galangal cell water

Testing an instrument: skin moisture tester, skin moisture loss tester.

The test scheme is as follows: after the tested subjects are screened to be qualified, the tested parts are cleaned by clean water and uniformly wiped by dry facial tissues. Marking the tested part with a 3cm by 3cm positioning card, testing the data of the moisture content of the skin cuticle and the transdermal water loss rate before using the sample after 20min of rest in a constant-temperature and constant-humidity environment, respectively sucking 30 mu L of the sample to the corresponding tested part with a liquid transfer gun, massaging for 60s with fingers, standing in a constant-temperature and constant-humidity chamber, and finally testing the data of the moisture content of the skin cuticle and the transdermal water loss rate 1h, 2h and 3h after the sample is smeared.

Subject screening conditions: healthy skin adults; the working environment is provided with an air conditioner; the subject is not sensitive to common cosmetics; the test site did not participate in other clinical trials at present or in the last three months;

limitation matters: during the trial period, the treatment for influencing the test on the tested part is forbidden; the use of other skin care products and other products that affect the test are prohibited; daily products such as shower gel, soap, shampoo and the like are consistent with those before the beginning of the trial, and are prohibited from being replaced.

The test results are shown in tables 3 and 4.

Table 3: data average of water content and water content improvement rate of stratum corneum of example 1 and comparative example 3

Through the data in table 3, the improvement rate of the water content of the stratum corneum within 3 hours after the sample of the galangal cell water in example 1 is higher than that of the blank group, which shows that the galangal cell water obtained by the method of the invention has certain moisturizing effect. The galangal cell water obtained by the method of comparative example 3 had insufficient effect of improving the water content of the skin stratum corneum and poor moisturizing effect.

Table 4: average values of data on the transdermal water loss rate and the transdermal water loss improvement rate of example 1 and comparative example 3

Through the data in table 3, the improvement rate of percutaneous water loss is higher than that of the blank group within 3h after the galangal cell water sample in example 1 is used, and the galangal cell water obtained by the method provided by the invention has the efficacy of repairing skin barriers and plays a role of moisturizing the skin. The galangal cell water obtained by the method of comparative example 3 was significantly less effective in improving the rate of percutaneous water loss.

Analysis of the process results of the examples and comparative examples:

table 1: content of main volatile active ingredient of galangal cell water extracted in examples and comparative examples

Continuing with Table 1:

by comprehensively analyzing the examples and the comparative examples, the extraction method can obtain the high-quality galangal cell water with more volatile active ingredient components and high content, has the special aromatic smell of galangal, avoids the spicy stimulation caused by the galangal, and has high safety.

As shown in comparative example 1, the extracted cell sap was low in weight, less in components and less in odor by using a single low-temperature vacuum extraction technique. As can be seen from comparative example 2, after a certain amount of enzyme and water are added to carry out enzymolysis on the galangal, the low-temperature vacuum technology is adopted to extract, so that the problem of foreign flavor caused by excessive enzymolysis can be solved; in addition, the water permeability is poor, and the added water can dilute the extracting solution, so that the defects of low extraction rate, light cell water aroma and the like are caused. As shown in comparative example 3, the galangal cell water obtained by the single enzyme extraction method contains more impurities and has heavy odor, and the extracting solution has low concentration and low value because 5kg of water is additionally added. As is clear from comparative example 4, since the initial extraction time was too short, the initial extraction cell liquid was small, and the initial extraction cell water was evaporated in less than 30 minutes when the cell liquid was again returned to the vessel for extraction, the degree of enzymatic hydrolysis was too low, the yield of the extracted cell water was not high as compared with that of example 1, and the active ingredient was small, resulting in a weak flavor.

Claims

1. A preparation method of galangal cell water is characterized by comprising the following steps: adding no solvent, primarily extracting galangal at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, condensing galangal cell water to form steam, collecting liquid, extracting for 1.5-2.5 hours to obtain primary extracted cell water and primary extracted galangal residue, adding 0.2-0.4 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary galangal into the primary extracted cell water, then pouring the mixture into the primary extracted galangal residue, extracting again at the temperature of 30-45 ℃ and under the pressure of-80 kPa to-101 kPa, and collecting galangal cell water after 3-7 hours of extraction.

2. The method for preparing galangal cell water according to claim 1, wherein the primary extraction temperature is 35 ℃ to 50 ℃ and the pressure is-80 kPa to-101 kPa.

3. The method for preparing galangal cell water according to claim 1, wherein the cellulase is added in an amount of 0.25 to 0.35%, and the pectinase is added in an amount of 0.01 to 0.06%.

4. The method for producing galangal cellular water according to claim 1, wherein stirring is performed during extraction at a speed of 1-150 rpm.

5. The method for preparing galangal cellular water according to claim 1, wherein the condensation is performed during the collection at a temperature of-10 ℃ to 8 ℃.

6. The method for producing galangal cell water according to claim 1, wherein galangal is cut into ginger pieces having a thickness of 1mm to 10 mm.

7. The method of claim 1, wherein the Alpinia officinarum is Alpinia officinarum rhizome.

8. Use of the cellular water of Alpinia officinarum Hance obtained by the method according to any one of claims 1 to 7, in the fields of food, health products, pharmaceuticals and cosmetics.