CN111454243A - Ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E - Google Patents

Ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E Download PDF

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Publication number
CN111454243A
CN111454243A CN202010269583.3A CN202010269583A CN111454243A CN 111454243 A CN111454243 A CN 111454243A CN 202010269583 A CN202010269583 A CN 202010269583A CN 111454243 A CN111454243 A CN 111454243A
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cucumber
weight
parts
vitamin
high pressure
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矫立勇
李红印
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Hebei Shengao Cosmetics Co ltd
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Hebei Shengao Cosmetics Co ltd
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Priority to CN202010269583.3A priority Critical patent/CN111454243A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/70Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with two hydrocarbon radicals attached in position 2 and elements other than carbon and hydrogen in position 6
    • C07D311/723,4-Dihydro derivatives having in position 2 at least one methyl radical and in position 6 one oxygen atom, e.g. tocopherols
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/18Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses an ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E, which comprises the following steps: preparing cucumber raw stock, preparing a cucumber raw stock light yeast solution, ultrasonically grinding to break the wall, homogenizing and breaking the wall under high pressure, extracting with alcohol, saponifying, extracting, freezing and concentrating to obtain the high-activity cucumber vitamin E. The invention develops a method for extracting vitamin E from cucumbers, greatly expands the sources of natural vitamin E, further improves the comprehensive utilization level of the cucumbers, and fully excavates the additional value of the cucumbers.

Description

Ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E
Technical Field
The invention relates to the technical field of plant extraction, in particular to an extraction process method of an antioxidant active ingredient in cucumber.
Background
Vitamin e (vitamine), also known as tocopherol (toeophanol), is widely used as a natural antioxidant in industrial products such as oil, food, cosmetics and the like, and can be used as a medical product for preventing diseases such as arteriosclerosis, cerebral hemorrhage, liver disease, diabetes and the like. VE cannot be metabolized and synthesized in human body, and can only be taken from outside, and the daily intake of ordinary people is 30 mg.
Vitamin E can be divided into natural vitamin E and synthetic vitamin E by its source. The natural vitamin E is easy to be absorbed by skin, can promote skin metabolism, prevent pigmentation, improve skin elasticity, and has special functions of caring skin, and preventing aging. Tests prove that the natural vitamin E is superior to the synthetic vitamin E in nutrition, physiological activity and safety. There are studies showing that: the physiological and antioxidant activity of the artificially synthesized vitamin E is only equal to 1/3 of natural vitamin E. In recent years, with the emphasis on food safety, many international organizations have struggled against the addition of chemically synthesized products to foods, and the demand of the market for natural vitamin E has been on rising year by year.
Consumers currently prefer to use natural antioxidants, with the annual demand for vitamin E alone as an antioxidant exceeding 15 million kg. The natural vitamin E is extracted from deodorized distillate in Japan, Europe and America, and the scale production in China is not available. Most of Chinese researches on natural VE focus on the extraction of deodorized distillates of soybean and rapeseed oil, and a small amount of reports on vitamin E extraction from malt and corn stigma exist, but the reports on the extraction of natural vitamin E from cottonseed oil in the flower melon are rare.
Disclosure of Invention
The invention aims to solve the technical problem of providing an ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
An ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E comprises the following steps:
A. preparing cucumber raw stock: cleaning fresh cucumbers, and pulping into cucumber raw pulp by using a food-grade pulping machine;
B. preparing cucumber original juice light yeast liquid: adding 10-20 parts by weight of brown sugar as a quick-acting carbon source into every 100 parts by weight of cucumber raw stock, immediately inoculating a flora consisting of bacillus subtilis and saccharomycetes, carrying out open aerobic fermentation, controlling the fermentation temperature to be 20-40 ℃, carrying out quick fermentation for 15-30h, finally adjusting the pH value to be neutral, and adjusting the water content to be 30-50% w/w to obtain the cucumber raw stock light fermentation liquid subjected to quick fermentation treatment;
C. ultrasonic grinding and wall breaking: placing the obtained cucumber original light yeast liquid in a mortar, placing quartz sand in the middle of the mortar, freezing, grinding into homogenate, and performing ultrasonic treatment on the homogenate for 1-3min by using 5-15kHz ultrasonic waves under the ice bath condition;
D. homogenizing the obtained material under 10-40MP pressure by liquid shearing and crushing device under high pressure for breaking wall for 5-15min, and controlling inlet and outlet temperatures at 20-40 deg.C and 25-40 deg.C respectively;
E. alcohol extraction: adding 2 parts by weight of anhydrous sodium sulfate into every 100 parts by weight of the materials obtained in the previous step, extracting with alcohol for 2-6 minutes, sealing, standing and layering to obtain an oil phase and an ethanol phase;
F. saponification: adding 1-2 parts by weight of ascorbic acid and 1-5 parts by weight of sodium hydroxide into an ethanol phase, introducing nitrogen, heating to boil and refluxing for 1-5 h;
G. and (3) extraction: adding 50-150 parts by weight of water and 100-300 parts by weight of normal hexane into the saponification solution, fully stirring, sealing and standing to obtain an ethanol phase and a normal hexane phase;
H. freezing and concentrating: separating precipitate at low temperature after freezing, and finally distilling and concentrating the n-hexane phase by using a rotary evaporator to obtain the concentrated cucumber vitamin E.
As a preferred technical scheme of the invention, in the step B, 15 parts by weight of brown sugar is added into every 100 parts by weight of the cucumber raw stock to serve as a quick-acting carbon source, a flora consisting of bacillus subtilis and saccharomycetes is immediately inoculated, the fermentation is carried out in an open aerobic fermentation mode, the fermentation temperature is controlled to be 30 ℃, the rapid fermentation is carried out for 20 hours, finally, the pH value is adjusted to be neutral, the water content is adjusted to be 35% w/w, and the cucumber raw stock light fermentation liquid subjected to the rapid fermentation treatment is obtained.
As a preferred technical scheme of the invention, in the step B, the bacillus subtilis and the microzyme are fully activated in brown sugar water at 30 ℃ before use, so that the number of viable bacteria reaches more than 260 hundred million/CFU; the weight ratio of the activated bacterial liquid to the cucumber raw stock is 1: 10.
And C, placing the obtained cucumber puree light yeast liquid in a mortar, placing quartz sand in the mortar, freezing, grinding into homogenate, and carrying out ultrasonic treatment on the homogenate for 2min by using 10kHz ultrasonic wave under the ice bath condition.
In the step D, the obtained cucumber raw stock light yeast liquid is subjected to high-pressure homogenization and wall breaking for 10min by a liquid shearing and crushing device under the pressure of 25MP, and the inlet temperature and the outlet temperature are respectively controlled at 30 ℃ and 35 ℃.
In the step E, 2 parts by weight of anhydrous sodium sulfate is added into every 200 parts by weight of the materials obtained in the previous step, alcohol extraction is carried out for 4 minutes, and the mixture is sealed, kept stand and layered to obtain an oil phase and an ethanol phase;
in the step F, 1.52 parts by weight of ascorbic acid and 35 parts by weight of sodium hydroxide are added into an ethanol phase, and nitrogen is introduced to heat the ethanol phase until the ethanol phase is boiled and refluxed for 2.5 hours;
in the step G, 100 parts by weight of water and 180 parts by weight of n-hexane are added into the saponification liquid, and the saponification liquid is fully stirred, sealed and kept stand to obtain an ethanol phase and an n-hexane phase.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: the method for extracting vitamin E from cucumber greatly expands the source of natural vitamin E and provides rich resources for extracting vitamin E. The invention provides a comprehensive extraction method combining mild fermentation, graded wall breaking, extraction and saponification, and the vitamin E is extracted from the cucumber, so that the comprehensive utilization level of cucumber products can be further improved, and a new way for improving the use potency of the cucumber is opened up.
Detailed Description
The following examples illustrate the invention in detail. The raw materials and various devices used in the invention are conventional commercially available products, and can be directly obtained by market purchase.
In the following description of embodiments, for purposes of explanation and not limitation, specific details are set forth, such as particular system structures, techniques, etc. in order to provide a thorough understanding of the embodiments of the present application. It will be apparent, however, to one skilled in the art that the present application may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present application with unnecessary detail.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It should also be understood that the term "and/or" as used in this specification and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items.
As used in this specification and the appended claims, the term "if" may be interpreted contextually as "when", "upon" or "in response to" determining "or" in response to detecting ". Similarly, the phrase "if it is determined" or "if a [ described condition or event ] is detected" may be interpreted contextually to mean "upon determining" or "in response to determining" or "upon detecting [ described condition or event ]" or "in response to detecting [ described condition or event ]".
Furthermore, in the description of the present application and the appended claims, the terms "first," "second," "third," and the like are used for distinguishing between descriptions and not necessarily for describing or implying relative importance.
Reference throughout this specification to "one embodiment" or "some embodiments," or the like, means that a particular feature, structure, or characteristic described in connection with the embodiment is included in one or more embodiments of the present application. Thus, appearances of the phrases "in one embodiment," "in some embodiments," "in other embodiments," or the like, in various places throughout this specification are not necessarily all referring to the same embodiment, but rather "one or more but not all embodiments" unless specifically stated otherwise. The terms "comprising," "including," "having," and variations thereof mean "including, but not limited to," unless expressly specified otherwise.
Example 1 preparation of cucumber puree light fermentation liquid
Cleaning fresh cucumbers, peeling, and pulping into cucumber raw pulp by using a food-grade pulping machine; adding 15 parts by weight of brown sugar into per 100 parts by weight of cucumber raw pulp as a quick-acting carbon source, immediately inoculating a flora consisting of bacillus subtilis and saccharomycetes, and fully activating the bacillus subtilis and the saccharomycetes in brown sugar water at 30 ℃ before use to enable the number of viable bacteria to reach more than 260 hundred million/CFU; the weight ratio of the activated bacterial liquid to the cucumber raw stock is 1:10, then the fermentation is carried out in an open aerobic way, the fermentation temperature is controlled at 30 ℃, the rapid fermentation is carried out for 20h, finally, the pH value is adjusted to be neutral, the water content is adjusted to 35% w/w, and the cucumber raw stock light fermentation liquid subjected to the rapid fermentation treatment is obtained.
Example 2 ultrasonic grinding-high pressure homogenization and fractionation for wall breaking
Placing the light fermentation broth of cucumber puree in a mortar, placing quartz sand in the middle of the mortar, freezing, grinding into homogenate, and performing ultrasonic treatment on the homogenate for 2min by using 10kHz ultrasonic wave under the ice bath condition; homogenizing the obtained cucumber raw stock light yeast liquid under 25MP pressure for breaking cell wall for 10min, and controlling the inlet and outlet temperatures at 30 deg.C and 35 deg.C respectively.
Example 3 alcohol extraction
Adding 2 parts by weight of anhydrous sodium sulfate into every 200 parts by weight of the materials obtained in the previous step, extracting with alcohol for 4 minutes, sealing, standing and layering to obtain an oil phase and ethanol.
Example 4 saponification
Adding 1.52 weight parts of ascorbic acid and 35 weight parts of sodium hydroxide into the ethanol phase, introducing nitrogen, and heating to boil and reflux for 2.5 h.
Example 5 extraction
Adding 100 parts by weight of water and 180 parts by weight of n-hexane into the saponification solution, fully stirring, sealing and standing to obtain an ethanol phase and an n-hexane phase.
Example 6 concentration
Washing with water for 1-2 times, freezing, separating precipitate at low temperature, and concentrating n-hexane phase by rotary evaporator to obtain concentrated cucumber vitamin E.
In summary, the above embodiments provide a new method for extracting vitamin E from cucumber, and the method combines a comprehensive process flow of mild fermentation, fractional wall breaking, extraction and saponification, and extracts vitamin E from cucumber, so that the comprehensive utilization level of cucumber products can be further improved, and a new way for improving the use potency of cucumber is opened up.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not substantially depart from the spirit and scope of the embodiments of the present invention, and are intended to be included within the scope of the present invention.

Claims (8)

1. An ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E is characterized in that: the method comprises the following steps:
A. preparing cucumber raw stock: cleaning fresh cucumbers, and pulping into cucumber raw pulp by using a food-grade pulping machine;
B. preparing cucumber original juice light yeast liquid: adding 10-20 parts by weight of brown sugar as a quick-acting carbon source into every 100 parts by weight of cucumber raw stock, immediately inoculating a flora consisting of bacillus subtilis and saccharomycetes, carrying out open aerobic fermentation, controlling the fermentation temperature to be 20-40 ℃, carrying out quick fermentation for 15-30h, finally adjusting the pH value to be neutral, and adjusting the water content to be 30-50% w/w to obtain the cucumber raw stock light fermentation liquid subjected to quick fermentation treatment;
C. ultrasonic grinding and wall breaking: placing the obtained cucumber original light yeast liquid in a mortar, placing quartz sand in the middle of the mortar, freezing, grinding into homogenate, and performing ultrasonic treatment on the homogenate for 1-3min by using 5-15kHz ultrasonic waves under the ice bath condition;
D. homogenizing and breaking walls under high pressure: homogenizing the obtained material under 10-40MP pressure by liquid shearing and crushing device under high pressure for breaking wall for 5-15min, and controlling inlet and outlet temperatures at 20-40 deg.C and 25-40 deg.C respectively;
E. alcohol extraction: adding 2 parts by weight of anhydrous sodium sulfate into every 100 parts by weight of the materials obtained in the previous step, extracting with alcohol for 2-6 minutes, sealing, standing and layering to obtain an oil phase and an ethanol phase;
F. saponification: adding 1-2 parts by weight of ascorbic acid and 1-5 parts by weight of sodium hydroxide into an ethanol phase, introducing nitrogen, heating to boil and refluxing for 1-5 h;
G. and (3) extraction: adding 50-150 parts by weight of water and 100-300 parts by weight of normal hexane into the saponification solution, fully stirring, sealing and standing to obtain an ethanol phase and a normal hexane phase;
H. freezing and concentrating: separating precipitate at low temperature after freezing, and finally distilling and concentrating the n-hexane phase by using a rotary evaporator to obtain the concentrated cucumber vitamin E.
2. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: and in the step B, adding 15 parts by weight of brown sugar into every 100 parts by weight of cucumber raw stock as a quick-acting carbon source, immediately inoculating a flora consisting of bacillus subtilis and saccharomycetes, carrying out open aerobic fermentation, controlling the fermentation temperature to be 30 ℃, carrying out quick fermentation for 20 hours, finally adjusting the pH value to be neutral, and adjusting the water content to be 35% w/w to obtain the cucumber raw stock light fermentation liquid subjected to quick fermentation treatment.
3. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: in the step B, before use, the bacillus subtilis and the microzyme are fully activated in brown sugar water at 30 ℃ so that the number of live bacteria reaches more than 260 hundred million/CFU; the weight ratio of the activated bacterial liquid to the cucumber raw stock is 1: 10.
4. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: and C, placing the obtained cucumber protoplasm light yeast liquid in a mortar, placing quartz sand in the mortar, freezing, grinding into homogenate, and carrying out ultrasonic treatment on the homogenate for 2min by using 10kHz ultrasonic wave under the ice bath condition.
5. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: in step D, performing high-pressure homogenization on the obtained cucumber raw stock light yeast liquid by a liquid shearing and crushing device under the pressure of 25MP for breaking the wall for 10min, and controlling the inlet and outlet temperatures at 30 ℃ and 35 ℃ respectively.
6. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: and step E, adding 2 parts by weight of anhydrous sodium sulfate into every 200 parts by weight of the materials obtained in the previous step, extracting with alcohol for 4 minutes, sealing, standing and layering to obtain an oil phase and an alcohol phase.
7. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: and step F, adding 1.52 parts by weight of ascorbic acid and 35 parts by weight of sodium hydroxide into the ethanol phase, introducing nitrogen, and heating to boil and reflux for 2.5 hours.
8. The ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E as claimed in claim 1, characterized in that: and G, adding 100 parts by weight of water and 180 parts by weight of normal hexane into the saponification liquid, fully stirring, sealing and standing to obtain an ethanol phase and a normal hexane phase.
CN202010269583.3A 2020-04-08 2020-04-08 Ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E Pending CN111454243A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2613661A (en) * 2021-12-13 2023-06-14 Blackswan Graphene Inc Homogenizer control system

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1069269A (en) * 1991-08-12 1993-02-24 童兴龙 Extract the method for natural VE from no phenol cotton oil
CN103467431A (en) * 2013-09-06 2013-12-25 中国农业科学院棉花研究所 Method for extracting vitamin E from cottonseed oil

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1069269A (en) * 1991-08-12 1993-02-24 童兴龙 Extract the method for natural VE from no phenol cotton oil
CN103467431A (en) * 2013-09-06 2013-12-25 中国农业科学院棉花研究所 Method for extracting vitamin E from cottonseed oil

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吕慧芳等: "黄瓜的保健价值及机理研究进展", 《吉林蔬菜》, pages 135 - 58 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2613661A (en) * 2021-12-13 2023-06-14 Blackswan Graphene Inc Homogenizer control system

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