CN115581266B - Clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice - Google Patents

Clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice Download PDF

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CN115581266B
CN115581266B CN202211070103.6A CN202211070103A CN115581266B CN 115581266 B CN115581266 B CN 115581266B CN 202211070103 A CN202211070103 A CN 202211070103A CN 115581266 B CN115581266 B CN 115581266B
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nanofiltration
momordica grosvenori
volume
microwave
microwave treatment
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CN115581266A (en
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李伟
黄华学
刘庚贵
吴国亮
唐美玉
黄�俊
贺进军
宋谷良
江小龙
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Hunan Huacheng Biotech Inc
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof containing fruit or vegetable juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof containing fruit or vegetable juices
    • A23L2/04Extraction of juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof containing fruit or vegetable juices
    • A23L2/08Concentrating or drying of juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof containing fruit or vegetable juices
    • A23L2/08Concentrating or drying of juices
    • A23L2/082Concentrating or drying of juices by membrane processes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/52Adding ingredients
    • A23L2/60Sweeteners
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/10Natural spices, flavouring agents or condiments; Extracts thereof
    • A23L27/12Natural spices, flavouring agents or condiments; Extracts thereof from fruit, e.g. essential oils
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/30Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
    • A23L5/34Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using microwaves
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Water Supply & Treatment (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention relates to a clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice, which comprises the steps of firstly preprocessing momordica grosvenori to reduce the water content to a certain degree, then carrying out microwave treatment, extracting lime water and CO 2 Neutralizing, excessive ceramic membrane, twice nanofiltration, and treating the trapped fluid of the twice nanofiltration to obtain the dry powder and concentrated juice of fructus Siraitiae Grosvenorii. The method is not applicable to adsorption resin and organic solvent, is a green and environment-friendly clean production method of the momordica grosvenori extract, can continuously and simultaneously obtain the momordica grosvenori extract products with two specifications, and has high product quality and good taste.

Description

Clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice
Technical Field
The invention relates to a production method of a momordica grosvenori extract, in particular to a clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice.
Background
Fructus Siraitiae Grosvenorii extract is prepared by scientific method. Currently, they are used primarily as natural, low-calorie, high-intensity sweeteners in functional food and beverage applications. The fructus Siraitiae Grosvenorii extract has sweet taste of mogroside 200-300 times of sucrose, wherein the sweetness of mogroside V can reach about 400 times of sucrose. The use standard of GB2760 food additives specifies that mogrosides can be used as sweeteners in various foods in an unlimited amount. Belongs to the range of 0 heat quantity, and can not cause blood sugar change and decayed tooth. The mogroside is used as a natural sweetener, has high sweetness, pure sweetness and taste close to sucrose. Has good solubility and stability, can be used from acidity to neutrality, and can be widely used in various foods and beverages. At present, the extraction process of the momordica grosvenori is a research and development hot spot of the momordica grosvenori industry.
Two types of fructus momordicae extracts currently on the market mainly comprise two forms: in order to remove impurities affecting taste and improve color of products in the production process of dry powder and concentrated solution, macroporous adsorption resin, ion exchange resin and the like are commonly adopted. The resin is used for purifying and separating the momordica grosvenori, so that a large amount of solvent is consumed, the cost is increased on one hand, and a large amount of waste liquid is generated on the other hand. In addition, although the resin can be regenerated, the regeneration of the resin requires consumption of chemicals such as strong base, strong acid, alcohol solvent, etc., which also increases the production cost. Therefore, a clean production method without resin, strong acid, strong alkali and organic solvent is urgently needed in the Momordica grosvenori processing industry, so as to solve the problem of increasingly serious environmental pollution and meet the increasingly strict international food additive production specification.
Microwave-assisted extraction is a novel natural product extraction technology, and can be carried out under milder conditions without using an organic solvent. The principle is that the plant cell wall is broken by microwaves, so that the extraction efficiency is increased.
CN104940537a discloses a preparation method of a momordica grosvenori compound extract, which is characterized in that momordica grosvenori is initially extracted by water, an extracting solution is used as a solvent to further extract tea compound, and then the momordica grosvenori compound extract is obtained by filtering, enzymolysis, decoloration, nanofiltration, concentration and drying. Wherein microwave-assisted extraction is used for the extraction of the tea leaf and tea leaf compound.
CN110339225a discloses a method for extracting fructus momordicae, which comprises the steps of freezing and crushing a fructus momordicae raw material, extracting freeze-dried powder by using petroleum ether, drying to obtain fructus momordicae powder, continuously extracting the fructus momordicae powder by using a high-alcohol solution under a microwave condition, and filtering and concentrating to obtain a fructus momordicae extract.
CN112121073a discloses a momordica grosvenori extract, which is obtained by extracting momordica grosvenori powder with water at 97-105 ℃ under boiling, extracting filtrate and ethyl acetate under microwave condition, and removing solvent by rotary evaporation.
CN111217880a discloses a preparation method for extracting momordica glycosides from momordica grosvenori, which uses the momordica grosvenori glycosides as an extraction solvent, extracts the momordica grosvenori under the auxiliary condition of microwaves, filters the momordica grosvenori, decolors the momordica grosvenori by using macroporous adsorption resin, and concentrates and dries the momordica grosvenori extract.
The prior art techniques described above all use microwave extraction techniques, but it can be seen that there are still some drawbacks, most of which are not completely free of the adsorption resin, and the use of organic solvents. Moreover, during microwave extraction, too high a power may damage the structure of mogroside, cause loss of the main sweet substance, or cause some other unknown changes, resulting in poor mouthfeel and taste of the obtained extract. This is contrary to the original purpose of the extract of Siraitia grosvenorii, i.e. the sensory experience of the extract of Siraitia grosvenorii should be considered before it is likely to be welcomed by consumers.
The inventor's prior patent CN202210918871.6 discloses a clean production method of momordica grosvenori extract, which optimizes the microwave extraction conditions, and is divided into two microwave extraction steps under different conditions, so that the yield of momordica grosvenori glycoside can be improved, and meanwhile, the taste of the momordica grosvenori product is considered. However, the yield of the mogroside V is low, and long-term practice shows that the portion of the permeate liquid of the nanofiltration membrane still contains a part of the mogroside, and the portion of the permeate liquid also contains a certain amount of small molecules such as glucose, fructose and the like. This part of permeate, if discarded, would result in waste of fructus Siraitiae Grosvenorii resources.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects in the prior art when preparing the high-quality momordica grosvenori extract, and provides a clean production method of the momordica grosvenori extract, which does not use resin for adsorption elution and organic solvents, has strong operability, is safe, green, environment-friendly and pollution-free, and is suitable for industrial production. On the basis of the prior technology of the applicant, the step of carrying out nanofiltration on the nanofiltration permeate liquid for the second time is added, and the obtained secondary nanofiltration retentate liquid is treated to obtain the fructus momordicae concentrated juice, so that on one hand, the yield of fructus momordicae V is further improved, on the other hand, two fructus momordicae extract products are obtained through serialization and clean process flow: momordica grosvenori dry powder and Momordica grosvenori concentrated juice.
The technical scheme adopted for solving the technical problems is as follows:
a clean production method of fructus Siraitiae Grosvenorii dry powder and fructus Siraitiae Grosvenorii concentrated juice comprises the following steps:
(1) Pretreatment: treating fresh fructus Siraitiae Grosvenorii to water content of 55-65%;
(2) Microwave treatment: pretreating fructus Siraitiae Grosvenorii by microwave treatment;
(3) Extracting lime water: crushing fructus Siraitiae Grosvenorii subjected to microwave treatment, stirring and extracting with dilute clarified lime water at room temperature, filtering, and centrifuging to obtain extractive solution;
(4) And (3) neutralization: introducing carbon dioxide gas into the centrifugate, and continuously stirring to generate fine precipitate and neutralizing liquid;
(5) And (3) ceramic membrane filtration: filtering the neutralization solution by using a ceramic membrane to obtain ceramic membrane filtrate;
(6) First nanofiltration: filtering the ceramic membrane filtrate with a nanofiltration membrane I, supplementing sufficient water to restore the original volume (namely the volume of the ceramic membrane filtrate) when the volume of the filtered trapped fluid is 1/4-1/5 of the volume of the ceramic membrane filtrate, and keeping the original filtering pressure and temperature to continue nanofiltration; until the volume of the trapped fluid is 1/4-1/5 of the volume of the ceramic membrane filtrate, respectively collecting nanofiltration trapped fluid I and nanofiltration membrane permeate I;
(7) Second nanofiltration: filtering the nanofiltration membrane permeation solution I by using a nanofiltration membrane II, supplementing sufficient pure water to the original volume when the volume of the trapped fluid is 1/15-1/20 of the original volume (the volume of the nanofiltration permeation solution I), and keeping the original filtration pressure and temperature to continue nanofiltration; until the volume of the trapped fluid is 1/9-1/10 of the original volume, after the second nanofiltration is finished, collecting nanofiltration membrane trapped fluid II, and discarding nanofiltration membrane permeate fluid II;
(8) Preparing fructus Siraitiae Grosvenorii extract: concentrating the nanofiltration trapped fluid I under reduced pressure to obtain concentrated solution I, and spray drying the concentrated solution I to obtain Siraitia grosvenorii extract dry powder; concentrating the nanofiltration membrane II trapped liquid under reduced pressure to obtain concentrated solution II, and sterilizing to obtain fructus Siraitiae Grosvenorii concentrated juice.
Preferably, in the step (1), the water content of the fresh fructus momordicae is 58.5-62.4% after pretreatment. The pretreatment method is ventilation drying, baking in an oven, etc., and is not particularly limited, as long as the moisture content of the fresh fructus momordicae is reduced to a specified range without damaging the active ingredients in the fructus momordicae. The water content of the fresh fructus momordicae is reduced to the range, so that the subsequent microwave treatment is convenient. The moisture content in the momordica grosvenori is too high, and the momordica grosvenori is easy to crack and the chemical structure of the active ingredient is damaged during microwave treatment, so that the yield of the mogroside is reduced; the moisture of the momordica grosvenori is too low, and the microwave treatment cannot play a role.
The purpose of the microwave treatment is to deactivate and inactivate various biological enzymes and proteins in the fresh fructus momordicae, and prevent browning caused by Maillard reaction, thereby ensuring light color of the extracting solution, filtrate and concentrated solution in each subsequent step, and omitting the impurity removal and decolorization procedures of the traditional technology which are necessary to use various resins and fillers; the second purpose of the microwave treatment is to enhance the extraction efficiency of the mogroside by microwaves, and the moisture between the cell wall and the cell gap of the momordica grosvenori and substances with stronger molecular polarity absorb the microwave energy during the microwave treatment, so that the extraction efficiency of the effective active ingredients in the momordica grosvenori is improved. In the past, in order to enhance the extraction efficiency and yield of the momordica grosvenori, a certain amount of cellulase, hemicellulase and pectase are generally added for enzymolysis and then extraction is carried out, but the enzymolysis (comprising enzymes contained in the momordica grosvenori) can degrade the mogroside to different degrees under proper conditions, so that the yield of the mogroside is lower. The invention realizes the effects of enzyme deactivation and extraction efficiency improvement through microwave treatment.
Preferably, the microwave treatment in the step (2) is performed on a microwave processor with an automatic material conveying crawler, the momordica grosvenori is placed on the conveying crawler, and the time of the microwave treatment of the momordica grosvenori is regulated by controlling the conveying speed of the crawler. The microwave treatment condition is that the microwave frequency is 2000-3000Hz, preferably 2200-2450Hz; the microwave power is 20-100KW, and the microwave treatment time is 2-10 minutes. The microwave power is not too high, the microwave treatment time is not too long, otherwise, the damage to the effective components in the momordica grosvenori is generated, and the quality of the momordica grosvenori extract is reduced.
More preferably, the step (2) adopts two microwave treatment stages, wherein the microwave power of the first microwave treatment stage is 20-50KW, the microwave treatment time is 5-8 minutes, and the humidity is 60-70RH%; the microwave power of the second microwave treatment stage is 70-100KW, the microwave treatment time is 1-2 minutes, and the humidity is 75-85RH%. The inventor finds that according to the above two or more microwave treatment stages, firstly, microwave treatment with low power, low humidity and long time is carried out; and then the microwave treatment with high power and high humidity and short time is carried out. Through the microwave treatment at the two different stages, the taste and flavor of the fructus momordicae extract are improved to a certain degree while the extraction efficiency of the fructus momordicae is ensured. The possible reasons are that the fresh fruit shells of the momordica grosvenori are hard, have specificity on the absorption of microwave energy, and are more beneficial to enzyme deactivation and extraction of sweet glycoside by adopting a treatment mode of weak to strong microwave power.
Preferably, in the step (3), the crushing is performed until the grosvenor momordica seeds are not crushed.
Preferably, in the step (3), the mass percentage concentration of the calcium hydroxide in the dilute clarified lime water is 0.05-0.10%, and the lime water is 4-10 times of the weight of the fresh fructus momordicae. One of the purposes of lime water extraction is that water-soluble components in the momordica grosvenori are easy to grow microorganisms at normal temperature and natural pH, so that materials are rancid and mogroside is degraded, but lime water is alkaline, and microorganisms are difficult to grow, so that the occurrence of the conditions can be effectively prevented; secondly, the fresh fructus momordicae is rich in a large amount of pectin, and the pectin can be coagulated and precipitated by the existence of calcium ions so as to be subjected to subsequent centrifugal separation; thirdly, biological enzymes and proteins in the fresh fructus momordicae can be denatured and precipitated under alkaline conditions, and the subsequent centrifugal separation is convenient. The effective components in the fructus momordicae extract, such as mogrosides, are stable under the alkaline condition and cannot be chemically changed.
Preferably, in the step (3), the extraction mode is continuous countercurrent extraction or intermittent multiple (2-5 times) extraction, the total time of extraction is 2-4 hours, and the extraction temperature is room temperature. One of the purposes of room temperature extraction is to avoid using high temperature before the protein of the fructus momordicae is thoroughly separated, and also to prevent Maillard reaction of the material, which leads to browning of the material; and the second purpose is to save steam energy.
Preferably, in the step (3), the centrifugation mode is horizontal screw centrifugation. The purpose of centrifugation is to remove pectin, proteins, and suspended plant fibers and other insoluble materials that have coagulated from the lime water extract.
Preferably, in the step (4), the pH value of the carbon dioxide gas regulating material is in a range of regulating the pH value to 7.5-9.0. One of the purposes is to react carbon dioxide with calcium ions in the centrate to produce a water-insoluble calcium carbonate precipitate, thereby removing a substantial amount of calcium ions; secondly, neutralizing the alkalinity of the centrifugate; and thirdly, the traditional liquid inorganic acid (hydrochloric acid, sulfuric acid and the like) is replaced by the neutralization of carbon dioxide gas, so that the use of non-food processing aids or non-food additives can be avoided, and the introduction of other ionic compounds can be avoided. If the pH value of the carbon dioxide is more than 9, the carbon dioxide is too little to be introduced, and the aim cannot be fully achieved; if the pH value regulated by carbon dioxide is less than 7.5, the carbon dioxide may be excessively introduced, and the generated calcium carbonate precipitate continuously reacts with the excessive carbon dioxide to generate calcium bicarbonate which is easily dissolved in water, so that calcium ions cannot be removed in a large amount.
Preferably, in the step (5), the filtration pressure of the ceramic membrane filtration is 0.02-0.1 Mpa, and the pore size of the ceramic membrane is 0.2-1 μm. The purpose of using ceramic membrane filtration is to remove calcium carbonate precipitate and other fine insoluble substances generated in the step (4), improve the clarity of the material and prevent pollution and blockage of subsequent nanofiltration membranes.
Preferably, in the step (6), the molecular weight cut-off of the nanofiltration membrane I is 3000-5000Da, the filtration pressure is 0.1-0.3 Mpa, and the nanofiltration temperature is 10-15 ℃. The purpose of the nanofiltration membrane is to permeate glucose, fructose and other small-molecule saccharides, inorganic salts, ions, water and the like in the ceramic membrane filtrate through the nanofiltration membrane, so that the content of mogroside in the nanofiltration membrane trapped liquid is improved. If the molecular weight cut-off of the nanofiltration membrane is too small or the filtration pressure is too low, the above purpose cannot be fully achieved; if the molecular weight cut-off of the nanofiltration membrane is too large or the filtration pressure is too high, excessive mogrosides can permeate the nanofiltration membrane, so that the quantity and the content of the dry powder of the fructus momordicae extract in the step (6) are low. In the step (6), pure water is supplemented and nanofiltration is continued in the nanofiltration process, so that the nanofiltration separation effect is more thorough and more remarkable; controlling the temperature in the nanofiltration process to be 10-15 ℃, one of the purposes is to prevent the breeding of microorganisms, thereby ensuring the yield of glycoside V and the good flavor of the product; and the second purpose is to prevent the nanofiltration membrane from being heated and expanded to influence the flux and the membrane separation effect due to the temperature rise caused by long-time high-speed operation of the liquid material.
Preferably, in step (7), the nanofiltration membrane II has a molecular weight cut-off of 200-500Da, the filtration pressure is 0.3-0.5 MPa, and the filtration temperature is 10-15 ℃. The purpose of using the nanofiltration membrane II is to permeate most of water and inorganic salt in the nanofiltration permeate I through the nanofiltration membrane II (a small amount of glucose, fructose and other small-molecule saccharides can also partially permeate), so that the content of mogroside in the retentate of the nanofiltration membrane II is increased, and the concentration of glycoside V, glucose and fructose in the concentrated juice of the momordica grosvenori is considered. If the molecular weight cut-off of the nanofiltration membrane II is too small or the filtration pressure is too low, the aim cannot be fully achieved; if the molecular weight cut-off of the nanofiltration membrane II is too large or the filtration pressure is too high, the mogroside molecules possibly penetrate the nanofiltration membrane II, so that the loss of glycoside V in the fructus momordicae concentrated juice product in the step (8) is caused.
Preferably, in the step (8), the sugar degree of the concentrated solution is 30-60brix, and the sugar degree of the concentrated solution II is 55-70brix.
The principle of the method of the invention is as follows:
according to the invention, the fructus momordicae is pretreated, so that the water content of the fresh fructus momordicae is controlled within a specific range, and then the microwave treatment under specific conditions is carried out, so that on one hand, the enzyme deactivation effect is realized, the degradation of the fructus momordicae endogenous enzyme to the mogroside is prevented, and the Maillard reaction which is frequently generated in the production of the conventional process of the fructus momordicae glycoside is not generated in the subsequent production process due to the inactivation of the enzyme and the denaturation of the protein, so that the color and the taste of the finished product of the extract are improved and improved; on the other hand, the structure of the cell wall and the cell membrane in the momordica grosvenori is changed to generate certain damage, but the structure of the active ingredients is not influenced, the extraction efficiency of the momordica grosvenori is improved, and then the fresh momordica grosvenori is extracted by using dilute lime water, so that the leaching of impurities can be effectively inhibited, and the degradation of mogroside by microorganisms is prevented; neutralization with carbon dioxide gas can remove a large amount of calcium ions; the obvious insoluble substances and impurities can be removed by centrifugation and ceramic membrane filtration, so that the materials are clear and transparent; finally, two nanofiltration membranes with different specifications are used for selectively intercepting or penetrating water-soluble components (stevioside, micromolecular sugar and the like) in the materials, and the trapped liquid of the two nanofiltration is concentrated (dried) to obtain two fructus momordicae extracts with different specifications: fructus Siraitiae Grosvenorii dry powder and fructus Siraitiae Grosvenorii concentrated juice.
The method has the beneficial effects that:
(1) The process is a clean process for producing the momordica grosvenori extract, the whole process flow does not use any type of resin and organic solvent, the operability is strong, the process is safe, green and environment-friendly, no pollution is caused, the process is suitable for industrial production, and the production cost is effectively reduced
(2) The process is also a continuous preparation process of the momordica grosvenori extract, can continuously obtain two momordica grosvenori extract products, namely the momordica grosvenori dry powder and the momordica grosvenori concentrated juice, improves the extraction rate of the momordica grosvenori sweet glycoside, and widens the end product range of the momordica grosvenori industry.
(3) The invention adopts a specific microwave treatment process, particularly carries out microwave treatment for two times in a sectional manner, and can simultaneously improve the extraction efficiency of the momordica grosvenori extract, the product quality and the yield of the momordica grosvenori glycoside V.
Drawings
FIG. 1 is a schematic diagram of a microwave processor with conveyor tracks for use in the present invention.
Detailed Description
The invention is further illustrated below with reference to examples.
The fresh momordica grosvenori used in the embodiment of the invention is purchased from Guangxi Guilin, wherein the mass percentage content of mogroside V is 0.49%; the ceramic membrane and the nanofiltration membrane used in the embodiment of the invention are purchased from Nanjing Fulinde environmental protection technology Co., ltd; wherein the pore diameter of the ceramic membrane is 0.3 μm. The raw materials or chemical reagents used in the examples of the present invention, unless otherwise specified, were obtained by conventional commercial means.
The microwave processor of the embodiment of the invention is ordered from Hubei Mingjian industrial microwave equipment Co, the microwave frequency is adjustable at 2000-3000HZ, and the microwave power is adjustable at 20-500 KW. The microwave processor is 10 meters in length and is provided with a conveying crawler for placing materials, a valve for controlling humidity and a pipeline. The structure is schematically shown in fig. 1: wherein 1 is a conveying crawler belt, 2 is a microwave treatment box body, 3 is a pipeline, and an air valve is arranged for controlling the humidity inside the microwave treatment box body.
The average water content of the momordica grosvenori is tested by randomly selecting 10 pretreated momordica grosvenori, testing the water content by a drying method and taking an average value.
The embodiment of the invention adopts a high performance liquid chromatography HPLC external standard method to detect the content of mogroside V.
Example 1
(1) Pretreatment: 500kg of selected and cleaned fresh fructus momordicae is taken and placed for 15 days under a ventilation condition at 25+/-2 ℃ until the average water content of the fresh fructus momordicae is 58.5%;
(2) Microwave treatment: the fructus momordicae pretreated in the step (1) is flatly paved on a conveying crawler belt of a microwave processor, so that no overlapping is ensured, more than 3cm gaps are reserved between the fructus momordicae, the fructus momordicae sequentially passes through a microwave processor I and a microwave processor II which are provided with the conveying crawler belt capable of controlling the internal humidity (the conveying crawler belt is provided with an extraction valve and a ventilation valve for realizing), the microwave treatment is carried out, the microwave frequency of the microwave processor I is 2300Hz, the microwave power is 36KW, the relative humidity is 65+/-5% RH, and the conveying speed of the crawler belt is controlled so that the time of the fructus momordicae passing through the microwave processor I is 6min; the microwave frequency of the microwave processor II is 2450Hz, the microwave power is 80KW, the relative humidity is 80+/-5% RH, and the crawler belt conveying speed is controlled to enable the time for the momordica grosvenori to pass through the microwave processor II to be 2min; obtaining the momordica grosvenori after microwave treatment;
(3) Extracting lime water: crushing fructus Siraitiae Grosvenorii with microwave until fructus Siraitiae Grosvenorii seeds are not crushed, extracting with 5000L of clarified lime water with concentration of 0.08wt% at room temperature under stirring (two times of extraction each for 1 hr), and coarse filtering with 200 mesh filter cloth bag to obtain lime water extractive solution; centrifuging lime water extract for 1h at 2000rpm to obtain a centrifugate;
(4) Gas neutralization: introducing carbon dioxide gas into the centrifugate, continuously stirring, and adjusting the pH value of the material to 8.5, wherein white fine precipitate is generated;
(5) And (3) ceramic membrane filtration: filtering the material after gas neutralization with ceramic membrane under the pressure of 0.05 Mpa to obtain about 4600L of ceramic membrane filtrate;
(6) First nanofiltration: filtering the ceramic membrane filtrate with nanofiltration membrane I with molecular weight cut-off of 3000Da, wherein the nanofiltration pressure is 0.2 Mpa, the nanofiltration temperature is 12 ℃, when the nanofiltration is carried out until the volume of the trapped fluid is about 900L, 3700L of pure water is supplemented, and the original filtration pressure and temperature are maintained for continuous nanofiltration; collecting nanofiltration membrane trapped fluid I until the volume of the trapped fluid is about 900L;
(7) Second nanofiltration: filtering the nanofiltration membrane I permeate (about 7400L) with nanofiltration membrane II with molecular weight cut-off of 500Da, wherein the nanofiltration pressure is 0.45 Mpa, the temperature is 14 ℃, and when the nanofiltration is carried out until the volume of the retentate is about 370L, 7000L of pure water is supplemented, and the original filtration pressure and temperature are maintained to continue nanofiltration; until the volume of the trapped fluid is about 370L, after the second nanofiltration is finished, collecting nanofiltration membrane trapped fluid II, and discarding nanofiltration membrane permeate II;
(8) Preparing fructus Siraitiae Grosvenorii extract: concentrating the nanofiltration membrane trapped liquid I under reduced pressure until the sugar degree of the material is 42.1 brix to obtain concentrated solution, spray drying the concentrated solution, wherein the air inlet temperature of the spray drying condition is 200 ℃, the air outlet temperature is 90 ℃, and the content of mogroside V is 45.37 percent; concentrating the nanofiltration membrane trapped liquid II under reduced pressure until the sugar degree is 66.9brix to obtain concentrated liquid II, and sterilizing the concentrated liquid II with UHT (140 ℃ for 5 s) to obtain 7.35kg of fructus Siraitiae Grosvenorii concentrated juice, wherein the content of mogroside V is 3.37%. The total yield of mogroside V is 91.96 percent.
Example 2
The other conditions were the same as in example 1, except that the pretreatment in step (1) was to treat fresh grosvenor momordica fruit to an average moisture content of 62.4%.
Example 3
Other conditions were the same as in example 1 except that in step (2), the microwave power of microwave processor I was 20KW and the microwave power of microwave processor II was 100KW.
Example 4
Other conditions were the same as in example 1 except that in step (2), the microwave power of the microwave processor I was 50KW and the microwave power of the microwave processor III was 70KW.
Example 5
The other conditions were the same as in example 1 except that in step (2), only one microwave processor was used for microwave treatment at a microwave frequency of 2450Hz, a microwave power of 36KW and a relative humidity of 65.+ -. 5% RH for 8min.
Example 6
The other conditions were the same as in example 1 except that in step (2), only one microwave processor was used for microwave treatment at a microwave frequency of 2450Hz, a microwave power of 80KW and a relative humidity of 75.+ -. 5% RH for 4min.
Comparative example 1
Other conditions are the same as in example 1, except that the fresh momordica grosvenori is directly subjected to the microwave treatment without the pretreatment of the step (1).
Comparative example 2
The other conditions are the same as in example 1, except that the pretreatment in step (1) and the microwave treatment in step (2) are not performed, and the extraction in step (3) is performed after the fresh momordica grosvenori is crushed.
Comparative example 3
The other conditions are the same as in example 1 except that the lime water of step (3) is replaced with hot water at 90 ℃.
Application example
The fructus Siraitiae Grosvenorii extract obtained in the above example was subjected to the tests of yield and taste.
The dried momordica grosvenori powder and the concentrated momordica grosvenori juice obtained in the example are diluted with purified water to prepare a solution with the same sweetness as that of the 3wt% sucrose aqueous solution, and 10 subjects taste the solution. And (3) comprehensively scoring subjective mouthfeel, taste and smell, wherein the scoring is carried out according to 5-score full score, 5-score indicates that the most mouthfeel and taste are optimal, and 1-score indicates that the mouthfeel and taste are worst. The results are shown in table 1 below:
TABLE 1 results of mogroside V yield and taste Performance test of Siraitia grosvenorii extract
As can be seen from the data in Table 1, the momordica grosvenori extract obtained by the invention has moderate content of the mogroside V, and the yield of the stevioside V is obviously improved. The invention simultaneously obtains the Siraitia grosvenorii extract products with two specifications through a continuous clean production process, wherein the Siraitia grosvenorii dry powder is white powder in appearance, and the solution is clear and transparent and is suitable for being directly used as a high-power sweetener; the fructus Siraitiae Grosvenorii juice concentrate can be diluted for direct reference or used as sweetener of other beverage. The method is green and environment-friendly, does not use resin columns such as adsorption and the like and organic solvents, is green and environment-friendly, has low cost, small occupied area of production equipment and simple operation, and is very suitable for the production process of the momordica grosvenori extract.

Claims (8)

1. A clean production method of fructus momordicae dry powder and fructus momordicae concentrated juice is characterized by comprising the following steps:
(1) Pretreatment: treating fresh fructus Siraitiae Grosvenorii to water content of 55-65%;
(2) Microwave treatment: the pretreated fructus momordicae is treated by microwaves; two microwave treatment stages are adopted, the microwave power of the first microwave treatment stage is 36-50KW, the microwave treatment time is 5-8 minutes, and the humidity is 60-70RH%; the microwave power of the second microwave treatment stage is 70-80KW, the microwave treatment time is 1-2 minutes, and the humidity is 75-85RH%;
(3) Extracting lime water: crushing fructus Siraitiae Grosvenorii subjected to microwave treatment, stirring and extracting with dilute clarified lime water at room temperature, filtering, and centrifuging to obtain extractive solution; the mass percentage concentration of calcium hydroxide in the dilute clarified lime water is 0.05-0.10%, and the consumption of the lime water is 4-10 times of the weight of the fresh fructus momordicae;
(4) And (3) neutralization: introducing carbon dioxide gas into the extracting solution, and continuously stirring to generate fine precipitate and neutralizing the solution;
(5) And (3) ceramic membrane filtration: filtering the neutralization solution by using a ceramic membrane to obtain ceramic membrane filtrate;
(6) First nanofiltration: filtering the ceramic membrane filtrate by using a nanofiltration membrane I, supplementing sufficient water to restore the original volume, namely the volume of the ceramic membrane filtrate, and keeping the original filtering pressure and temperature to continue nanofiltration when the volume of the filtered trapped fluid is 1/4-1/5 of the volume of the ceramic membrane filtrate; until the volume of the trapped fluid is 1/4-1/5 of the volume of the ceramic membrane filtrate, respectively collecting nanofiltration trapped fluid I and nanofiltration membrane permeate I; the molecular weight cut-off of the nanofiltration membrane I is 3000-5000Da, the filtration pressure is 0.1-0.3 Mpa, and the nanofiltration temperature is 10-15 ℃;
(7) Second nanofiltration: filtering the nanofiltration membrane permeation solution I by using a nanofiltration membrane II, supplementing enough pure water to the original volume when the volume of the filtered trapped fluid is 1/15-1/20 of the volume of the nanofiltration permeation solution I, and keeping the original filtering pressure and temperature to continue nanofiltration; until the volume of the trapped fluid is 1/9-1/10 of the original volume, after the second nanofiltration is finished, collecting nanofiltration membrane trapped fluid II, and discarding nanofiltration membrane permeate fluid II; the molecular weight cut-off of the nanofiltration membrane II is 200-500Da, the filtration pressure is 0.3-0.5 Mpa, and the filtration temperature is 10-15 ℃;
(8) Preparing fructus Siraitiae Grosvenorii extract: concentrating the nanofiltration trapped fluid I under reduced pressure to obtain concentrated solution I, and spray drying the concentrated solution I to obtain Siraitia grosvenorii extract dry powder; concentrating the nanofiltration membrane II trapped liquid under reduced pressure to obtain concentrated solution II, and sterilizing to obtain fructus Siraitiae Grosvenorii concentrated juice.
2. The clean production method according to claim 1, wherein in the step (1), the fresh fructus momordicae is pretreated to have a water content of 58.5-62.4%.
3. The clean production method according to claim 1, wherein in the step (3), the crushing is performed so as not to crush the seeds of the momordica grosvenori.
4. The method according to claim 1, wherein in the step (3), the extraction is performed in a continuous countercurrent extraction or intermittent multiple extraction, the total time of extraction is 2-4 hours, and the extraction temperature is room temperature; the centrifugal mode is horizontal screw centrifugation.
5. The method according to claim 4, wherein in the step (3), the number of times of the plurality of extractions is 2 to 5.
6. The method according to claim 1, wherein in the step (4), the carbon dioxide gas is introduced in an amount to adjust the pH of the material in the range of 7.5 to 9.0.
7. The clean production method according to claim 1, wherein in the step (5), the filtration pressure of the ceramic membrane filtration is 0.02 to 0.1 Mpa, and the pore size of the ceramic membrane is 0.2 to 1 μm.
8. The clean production method according to claim 1, wherein in the step (8), the sugar degree of the concentrated solution I is 30-60brix, and the sugar degree of the concentrated solution II is 55-70brix.
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