WO2022110519A1 - 一种改善罗汉果提取物持久甜味的复配甜味剂及其制备方法 - Google Patents

一种改善罗汉果提取物持久甜味的复配甜味剂及其制备方法 Download PDF

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WO2022110519A1
WO2022110519A1 PCT/CN2021/072429 CN2021072429W WO2022110519A1 WO 2022110519 A1 WO2022110519 A1 WO 2022110519A1 CN 2021072429 W CN2021072429 W CN 2021072429W WO 2022110519 A1 WO2022110519 A1 WO 2022110519A1
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okra
sweetness
han guo
luo han
compound sweetener
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PCT/CN2021/072429
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English (en)
French (fr)
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刘庚贵
黄华学
曾润清
何安乐
黄�俊
陈明明
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湖南华诚生物资源股份有限公司
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Publication of WO2022110519A1 publication Critical patent/WO2022110519A1/zh

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30—Artificial sweetening agents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30—Artificial sweetening agents
    • A23L27/33—Artificial sweetening agents containing sugars or derivatives
    • A23L27/34—Sugar alcohols
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • the invention relates to the technical field of plant extraction and separation and the field of compound sweetener, in particular to a compound sweetener for improving the lasting sweetness of Luo Han Guo extract and a preparation method thereof.
  • the Luo Han Guo extract is prepared from the fresh ripe fruit of the Cucurbitaceae plant Luo Han Guo, which is first saccharified and then ripened, and then prepared through a series of separation and extraction steps.
  • Luo Han Guo extract has the best taste among all natural sweet substances and is the closest to sucrose. It has the significant advantages of refreshing sweetness, high sweetness and low calorie of sucrose. It does not change blood pressure and blood sugar, and does not cause dental caries. It is especially suitable for It is an ideal sugar substitute for people with diabetes, high blood pressure, obesity and those who are not suitable for sugar consumption. It is also an ideal sugar substitute for healthy people.
  • sucrose is a sweet taste in the mouth, reaching the peak sweetness in about 1-2 seconds and disappearing in about 5 seconds, which is the most ideal sweet taste at present. But at present, whether it is synthetic or natural high-intensity sweeteners, the problem is that the aftertaste is too heavy, which affects the taste.
  • the Luo Han Guo extract mainly includes: (1) Luo Han Guo powder, the preparation process of which mainly includes crushing, extraction, filtration, concentration, drying, etc., wherein the content of Mogroside V is 0.5 to 4%; (2) V25 to 35 Mogroside, its The preparation process mainly includes the steps of crushing, extraction, filtration, clarification, chromatography, concentration, drying, etc., wherein the mogroside V content is 25-35%; (3) V50 mogroside, the preparation process mainly includes crushing, extraction, filtration , clarification, chromatography, decolorization, desalination, concentration, drying and other steps, wherein the mogroside V content is 50-60%; (4) Momordica grosvenori concentrated juice, its preparation process mainly includes crushing, extraction, filtration, clarification, decolorization, desalination , concentration and other steps, wherein the mogroside V content is 0.5-5%.
  • the present invention does not relate to it, but mainly relates to the Luo Han Guo extract in a solid form.
  • Luo Han Guo extracts all have certain defects: (1) Luo Han Guo powder, V25 ⁇ 35 Mogroside: 1% aqueous solution is turbid, or has obvious post-precipitation phenomenon, which limits the use in beverages and other end products that require clarity (2) Luo Han Guo powder: without separation and purification, most of the substances originally stored in fresh Luo Han Guo are retained. Although the sweetness is close to saturation, it has no thick taste and still has a lasting sweetness, which is only higher than that of high content Luo Han Guo.
  • glucoside The duration of glucoside is short, and its sweetness lasts for about 25 seconds; the sweetness is slightly higher, about 14 times that of sucrose; (3) V25 ⁇ 35 mogrosides: After separation and purification, the mogrosides originally stored in fresh monk fruit are removed. Most of the substances lead to unsaturated sweetness and no thick taste. It has obvious lasting sweetness, and its sweetness lasts about 45 seconds; its sweetness is high, about 100 times that of sucrose; (4) V50 Mogroside : After separation and purification, most of the substances originally stored in fresh Luo Han Guo have been removed, resulting in unsaturated sweetness and no thick taste, with obvious lasting sweetness, and its sweetness lasts about 45 seconds; high sweetness, It is about 200 times that of sucrose.
  • Mogroside V in Luo Han Guo extract is an ideal high-power natural sweetener, but its role in various sweeteners is restricted due to the severe sweetness afterward.
  • Okra also known as lady's finger, coffee yellow sunflower, and tomato
  • Okra is the young fruit of the Malvaceae plant coffee yellow sunflower. Its edible part is the pod, which is divided into two kinds of green and red; its crisp, tender and juicy, Smooth and not greasy, unique fragrance, is loved by many people; it has the effects of sore throat, drenching, breast milk, and menstrual regulation; commonly used for sore throat, urination, sparse postpartum milk, and irregular menstruation.
  • the main ingredients of okra are:
  • Okra has a special mucus, which has the highest viscosity in the tender fruit 5 days after flowering.
  • the mucus is an important evaluation index for the quality of okra.
  • the main components are carbohydrate compounds, including pectin, polysaccharide and glycoprotein.
  • Okra pectin The content of okra pectin was the highest in tender fruit pods, followed by tender fruit seeds and mature fruit pods, accounting for 20.97%, 9.34% and 8.91%, respectively.
  • the protein content of okra is more, fresh fruit 2.3%, mature fruit 3.15%, and seeds 28.1%; amino acids are complete, and 17 species have been isolated and identified.
  • Okra is rich in VC , B family, VA, VE , and VK .
  • Each 100 grams of okra fresh fruit contains VA 198 ⁇ g , VB1 0.2mg, VB2 0.06mg, VC 44mg , VE 1.03mg, with more VC and VE content.
  • Okra is rich in mineral elements and contains 13 kinds of trace elements. According to the highest content (mg/100g) determined, they are K 95, Ca 343, P 65, Mg79.36, Mn 56.4, Zn 38.9, Cu 26.2, Se 11 , Fe 2.71, Cr 0.410, Pb 0.745, Cd 0.319.
  • Okra is rich in flavonoids and phenolic acid compounds, and the total amount of flavonoids in the fruit is 2.8%.
  • 12 flavonoid components have been isolated and identified, namely quercetin-3-O-diglucoside, myricetin-3- O-glucoside, quercetin-3-O-glucose-xyloside, quercetin-3-O-rutinoside, quercetin-3-O-glucoside, isorhamnetin-3-O-glucoside -Penttoside, quercetin-3-O-(malonyl)glucoside, myricetin-3-O-rhamnoside, 4,5,7-trihydroxyflavonoid-O-glucoside, myricetin , 4,5,7-trihydroxyflavone and quercetin.
  • Luo Han Guo extract used is mainly Mogroside, and mainly Mogroside with a content of more than 50% of Mogroside V, and it does not involve Luo Han Guo powder and other Luo Han Guo extracts that only have a lower content of Mogroside V, and has not passed through special plants. Extracts to alter the sweetness duration and sweetness fold of Luo Han Guo extracts.
  • CN201610005411.9 discloses a sweetener that changes the time profile of mogroside sweetness and its preparation method, but the effect of the patent is not ideal.
  • the inventors have proved through experiments that the addition of rutin did not increase the entrance sweetness of the mogroside aqueous solution, but increased the bitter taste; while shortening the sweetness time, it also enhanced the bitter taste, and the shorter the shortening time, the better the bitter taste. The more pronounced the bitterness, the more unacceptable the taste is.
  • the patent does not change the sweetness multiple of mogroside.
  • CN201910902694.0 discloses a compound sweetener of Luo Han Guo for stabilizing blood sugar and a preparation method thereof
  • CN201810374254.8 discloses a low-sugar caramel flavor composition containing mogroside, preparation method and application
  • CN201710035875.9 discloses a preparation method of healthy mogroside with double sugar or multiple sugar, belonging to the technical field of food
  • CN201410365736.9 discloses A Luo Han Guo drink with a low glycemic index
  • CN200510055228.1 discloses a sweetener added with Luo Han Guo extract and a preparation method thereof
  • CN200410022754.3 discloses a low-calorie Luo Han Guo sugar
  • CN201911372029.1 discloses a natural Compound sweetener and preparation method thereof
  • CN201910548599.5 discloses a production method of compound sweetener, and relates to the technical field of food additive production
  • CN201910322941.X discloses low-calorie compound sweetener and preparation thereof method
  • CN201310616422.7 discloses a natural compound sweetener and a preparation method thereof.
  • Luo Han Guo compound sweetener is all adding one or more sweeteners on the basis of Luo Han Guo extract, such as stevioside, psicose, sucralose, etc.; there are many kinds of substances, such as sugar Alcohols, mannose, etc., cannot highlight the excellent properties of some materials; they are prepared by simple processes, such as mixing, drying, or granulation, drying, etc., and it is difficult to achieve uniform composition inside and outside. There are common problems that the composition is complex, the effect is not obvious, and the defects of some materials are obvious.
  • the compound sweetener of Luo Han Guo lacks a special fragrance, and the compound sweetener composition often lacks this part of the fragrance, thick taste, and sweetness saturation; (6)
  • the preparation process is simple, and the additives in the formula are added.
  • the reason that causes the difficult problem that the compound sweetener of Luo Han Guo on the market is easy to harden is generally present, and the existing solution mainly prevents the compound sweetener of Luo Han Guo containing erythritol by filling the packaging bag with an inert gas.
  • Hardening the hardening problem has not been fundamentally solved from the perspective of composition, so that users will inevitably encounter hardening during use and affect the use, and the quality needs to be improved. None of the above prior art can effectively improve the after-sweetness problem of Mogroside V.
  • the technical problem to be solved by the present invention is to overcome the problem in the prior art based on the extract of Luo Han Guo, especially the problem that the sweetness of Mogroside V affects the mouthfeel, and to expand the application of the extract of Luo Han Guo as a natural high-sweetness sweet substance scope.
  • the Luo Han Guo powder, V25-35 mogroside, and V50 mogroside in the Luo Han Guo extract are used as high-sweet substances; the okra extract is used as the material to improve the taste, and the combination with the Luo Han Guo extract produces a synergistic effect. , which can not only shorten the sweetness duration of Mogroside V, but also bring a special aroma to the compound sweetener after a specific baking procedure.
  • the compound sweetener for improving the lasting sweetness of the Luo Han Guo extract provided by the invention obtains a product with the best comprehensive taste from the three aspects of smell, thick taste and sweetness saturation, so that the sweetness of the obtained Luo Han Guo compound sweetener is improved.
  • the smell lasts less than 10 seconds.
  • the Luo Han Guo compound sweetener provided by the invention has the same taste, mouthfeel and sweetness duration as sucrose, low-calorie, pure natural, special and pleasant fragrance of fruits and vegetables, and can be used as an ideal sugar substitute product for various groups of people.
  • the inventors of the present application have found through a large number of experiments and comparisons that when the sweetness of the sweetener solution of the present invention is close to that of the 5% sucrose solution, the sweetness of the sweetener solution of the present invention disappears within 10 seconds, and it can be used as an ideal sweetener.
  • a compound sweetener for improving the lasting sweetness and sweetness multiple of Luo Han Guo extract including raw materials: okra young fruit mucilage, okra concentrated juice, and Luo Han Guo extract , erythritol, provided that the quality of mogroside V in the Luo Han Guo extract is 0.3-1% of the total quality of the mucilage of young okra and the concentrated okra juice.
  • the compound sweetener comprises the following raw materials by mass: 30-50 parts of okra young fruit mucilage, 15-25 parts of okra concentrated juice, 1-30 parts of Luo Han Guo extract, 100-500 parts of red thritol.
  • the mass of mogroside V in the Luo Han Guo extract is 0.5-0.8% of the total mass of okra young fruit mucilage and okra concentrated juice.
  • Erythritol can be adjusted in a wide range of 100-500 parts, and the purpose is to obtain sweetener products with different sweetness according to demand, provided that the sweetness of compound sweeteners does not exceed ten times that of sucrose. More ideally, the sweetness of the compound sweetener is 1-6 times that of sucrose.
  • the content of solids in the mucilage of young okra fruit is 2-10%, preferably 4-7%; the content of solids in the concentrated okra juice is 20-30%.
  • the mucilage of the young okra fruit used in the present invention is obtained by a preparation method comprising the following steps: extracting the young okra fruit with water, collecting the extraction residue and the extract, and filtering the extract and concentrating to obtain the okra mucus.
  • the young okra fruits are harvested 4 to 7 days after the flowers fade, and the standard is as follows: first, it is necessary to ensure that the pods are tough, bright in color, swollen and not aged.
  • the harvesting standard of okra varies with temperature. At high temperatures, the length of the okra pods is about 10 cm, and when the temperature is low, the length is only about 8 cm. The length of the pods should be kept within 10 cm. Only young okra is rich in mucilage and has a special fruit and vegetable fragrance. As the fruit matures, the mucus content plummets, and the ripe okra can no longer be chewed.
  • the extraction temperature is 8-30°C, preferably 8-15°C.
  • the advantage of maintaining a lower extraction temperature is to maintain the excellent performance of the original ecological fruit and vegetable fragrance and thick taste of the okra concentrated juice, maintain the stability of the okra mucus colloid solution, and prevent the high temperature from destroying the stability and color enhancement of the colloid solution.
  • the quality of the water used in the extraction is 8-15 times the quality of the okra young fruit, preferably multiple extractions, such as two, three, and four extractions, and the amount of water used for each extraction decreases successively, and the amount of the decrease does not exceed 20% of the last extraction with water.
  • the filtration and concentration are not particularly limited, and conventional filtration and concentration methods in the art can be used.
  • the filtration is ceramic membrane filtration, and the ceramic membrane material is alumina or zirconia, and the pore size is 300-500nm; the concentration is reverse osmosis.
  • the membrane is concentrated to a solid content of 1-5%. Because the mucilage of okra young fruit has a certain viscosity, excessive concentration may lead to the concentration effect of the reverse osmosis membrane.
  • the okra concentrate used in the present invention is obtained by a preparation method comprising the following steps: taking the extraction residue in the preparation process of okra young fruit mucilage, baking to obtain flavor residue, extracting the flavor residue with an aqueous alcohol solution, filtering, and decolorizing , concentrated to obtain okra concentrate.
  • the roasting is carried out at 130-140° C. to obtain a burnt aroma, and the roasting time is 0.5-1.5 h.
  • the inventor found that when baking is carried out within the above temperature range, a series of complex chemical changes have occurred in the extraction residue, which can produce a strong coke aroma. It can not only shorten the sweetness time of the compound sweetener, and obviously improve the problem of serious after-sweetness of the sweetener compounded by the Luo Han Guo extract, but also bring a special fruit flavor.
  • dehydration is performed at a lower temperature, that is, at 65-100° C., to reduce the water content of the extraction residue to below 30%. More preferably, in the dehydration treatment, the extraction slag is first baked at 60-70°C for 0.5-1h to make the water content below 50%, and then baked at 90-100°C for 0.5-1h to make the water content within 50%. 30% or less.
  • the aroma of okra can be significantly increased by pretreatment and baking treatment, which can significantly increase the fruit and vegetable flavor and burnt flavor of okra.
  • the volume concentration of alcohol is 60-80%, preferably an aqueous solution of ethanol.
  • the steps of filtration, decolorization, and concentration are well known in the art.
  • the filtration is through a ceramic membrane to obtain a clear liquid; It has a certain concentration effect, and is concentrated to a solid content of 5-10%; the concentration is vacuum concentration, and concentrated to a solid content of 20-30%.
  • the advantage of vacuum concentration is that it can reduce the loss of fresh and burnt aroma of okra fruits and vegetables.
  • the Luo Han Guo extract can be divided into different specifications according to the content of Mogroside V in the extract, and can generally be divided into (1) Luo Han Guo powder (mogroside V content 0.5-4%) from the point of view of commodity availability; (2) V25-35 Mogroside (Mogroside V content 25-35%); (3) V50 Mogroside (Mogroside V content 50-60%).
  • the addition amount of the Luo Han Guo extract needs to satisfy that the quality of the mogroside V in the Luo Han Guo extract is 0.3-1% of the total mass of the mucilage of the young okra and the concentrated okra juice, preferably, the quality of the mogroside V in the Luo Han Guo extract is 0.3-1%. It is 0.5-0.8% of the total mass of okra young fruit mucilage and okra concentrate juice.
  • the inventor unexpectedly found that, with the extraction concentrate of okra young fruit mucilage and okra mucilage extract residue after baking treatment, and Luo Han Guo extract, the concentration of Mogroside V, the main sweet substance in the Luo Han Guo extract, was compounded.
  • the mass accounts for a certain content of the total mass of okra young fruit mucilage and okra concentrated juice, which can effectively shorten the after-sweetness of Mogroside V, and solve the problem of after-sweetness of Luohanguo extract as a high-intensity sweetener.
  • the sweetener has a special fruity aroma and tastes good.
  • the sweet compounding agent provided by the invention is mainly compounded with auxiliary materials from okra, which is cheap and easy to obtain, and is a compounded sweetener product with great market competitiveness.
  • the invention also provides the preparation method of the compound sweetener for improving the persistent sweetness and sweetness multiple of the Luo Han Guo extract, comprising the following steps: decolorizing the okra mucilage, the okra decolorized flavor concentrated juice, the Luo Han Guo extract, the erythromycin
  • the sugar alcohol is mixed in a certain proportion, dissolved, filtered, crystallized, granulated by boiling, and dried.
  • the crystals obtained by crystallization are dried to a moisture content of ⁇ 15% prior to boiling granulation.
  • the dissolving temperature is 5-15° C.
  • the volume of water added is 2-15 times the weight of erythritol (V/W).
  • a lower temperature is used for dissolving, in order to make the precipitation and post-precipitation of the mixed solution system as complete as possible, while erythritol does not precipitate, which is beneficial to the removal of precipitation and post-precipitation.
  • the precipitation and post-precipitation of the solution system can be completely removed, and a solution without precipitation and post-precipitation can be obtained under low temperature and normal temperature conditions.
  • the filtration adopts a ceramic membrane, which is made of alumina or zirconia, and the pore size of the ceramic membrane is 50-200 nm.
  • one-step crystallization or fractional crystallization can be adopted, and the method of fractional crystallization is preferably adopted.
  • the clear liquid of the ceramic membrane is first concentrated to a solid content of 30-40%, and then a uniform mixture crystal is precipitated under room temperature; .
  • This crystallization method can obtain a mixture crystallization that is evenly mixed, completely consistent inside and outside, and has crystalline luster.
  • the obtained crystals are first dried to a moisture content of ⁇ 15%, and the drying method is well known in the art, such as vacuum drying and blast drying.
  • the drying method is well known in the art, such as vacuum drying and blast drying.
  • the crystal obtained by crystallization is used as the carrier, and the obtained crystallization mother liquor is used as the injection liquid.
  • the boiling granulation method can avoid the addition of binder or water, maintain the original crystal form, and make the crystallization mother liquor and crystals fully and completely mixed evenly, and the crystallization mother liquor is mainly in the outer layer, in which erythritol and other
  • the combination of substances prevents the hardening of the crystalline particles in the post-drying period.
  • the crystalline carrier is required to be dried to a moisture content of less than or equal to 15%. In this way, the problem of product hardening in the air can be avoided. If the moisture content is too high, it is easy to dissolve and change the crystal form during the heating process, resulting in inconsistent crystal form; and also lead
  • the drying temperature is 55-65°C; the drying method is blast drying, or vacuum drying, or microwave vacuum drying, or belt vacuum drying, and the degree of vacuum is less than -0.085MPa.
  • Okra is rich in mucus, which can be dissolved in water even at low temperature. Therefore, by controlling the appropriate amount of water and the number of extractions, these components can be completely extracted and the unique fragrance of fruits and vegetables of okra is preserved. If the temperature is too high, these components are easily destroyed, and an unstable colloidal solution is formed, thereby destroying the stability of the solution, making it difficult to separate and purify the mucus, and unable to significantly increase the thick taste. After removing most of the mechanical impurities by centrifugation and then clarifying by microfiltration through a ceramic membrane, a clear mucus-rich solution can be obtained.
  • the pigment with molecular steric hindrance and the mucus with a very large molecular weight are separated under normal temperature conditions, thereby preparing the decolorized mucus of okra.
  • the extraction residue obtained by water extraction of okra still has some substances that are not extracted by the low-temperature aqueous solution. Under certain conditions, these substances can be baked to emit a strong fruit and vegetable fragrance and burnt fragrance, and this fragrance Consistent with the smell of roasted fresh okra. Therefore, the okra mucus is first extracted at low temperature, and then the extraction residue is flavored and flavored, so that not only good quality and stable mucus can be obtained, but also the unique rich fruit and vegetable fragrance and burnt flavor of okra can be obtained. In order to fully extract the components in the water-extracted residue, these components can be extracted at a lower temperature with a certain concentration of hydrous alcohol without losing the aroma components. Then, a small amount of impurities and precipitates are removed by the microfiltration clarification technology of ceramic membrane, and the concentrated juice of okra flavor is prepared by reverse osmosis membrane and vacuum decompression concentration.
  • This crystallization method precipitates most of the crystals in the mixture, and ensures the perfect crystal shape, luster and compositional uniformity of the crystals.
  • the moisture content of the crystal is controlled by drying, and the crystal is used as a carrier, and the boiling granulation technology is used to control the wind speed and temperature, so that the crystal and the mother liquor are combined again.
  • the mother liquor is sprayed regularly and uniformly during the boiling granulation process, thereby obtaining a good quality Luo Han Guo compound sweetener crystal.
  • the main component in the mother liquor comes from okra, it has a certain degree of hydrophobicity, which is complementary to the non-hygroscopic property of erythritol, which significantly changes the hardening time of the erythritol compound sweetener and makes the product use more convenient.
  • Luo Han Guo extract whether it is Luo Han Guo powder, or V25 ⁇ 35 and V50 Mogrosides, all have persistent sweetness, but the sweetness duration is somewhat different, ranging from 25 seconds to 45 seconds; they are all natural high-efficiency sweeteners , but due to the different content of mogroside V, its sweetness is 15 times to 200 times that of sucrose.
  • the young fruit of okra is rich in mucus, which is a kind of sugar polymer.
  • the main components are pectin, soluble dietary fiber, hydroxymethyl cellulose, etc., which makes its solution have a thick taste.
  • it is rich in protein and amino acids, and has a special fragrance of fruits and vegetables.
  • These special ingredients make okra mucilage and its extract have special effects: that is, it can increase the thick taste of the Luo Han Guo extract solution, improve the sweetness saturation, and through the special pleasant smell, synergistic effect, greatly improve Luo Han Guo The long-lasting sweetness of the extract, and the sweetness multiple is appropriately reduced.
  • Erythritol has a refreshing sweet taste. As a bulking low-intensity sweetener, it can further improve the lasting sweetness of Luo Han Guo extract on the basis of okra, and significantly reduce the sweetness multiple. Erythritol is easy to crystallize. Although it does not absorb moisture, compound sweeteners mainly containing erythritol are easy to harden, which is a difficult problem. The concentrated juice prepared from okra mucus and okra alcohol extraction can significantly delay the hardening time of erythritol to a certain extent, making it difficult to harden, which is also the result of interaction.
  • the corresponding ratio is controlled, and the sweetness duration of Luo Han Guo extract is shortened from 45 seconds to less than 10 seconds, thereby preparing a compound sweetener with improved lasting sweetness of the Luo Han Guo extract.
  • the present invention provides a compound sweetener for improving the lasting sweetness of the Luo Han Guo extract.
  • the thick and thick taste is increased by the mucilage of the young okra fruit, and the okra concentrated juice prepared by the aroma-enhancing process and the water-alcohol extraction increases the sweetness and saturation.
  • Aspects synergistically improve the long-lasting sweetness of the Luo Han Guo extract; and further improve the long-lasting sweetness of the Luo Han Guo extract through the low sweetness and refreshing taste of erythritol, and dilute the sweetness multiple.
  • the bitterness, taste, and sweetness duration of the Luo Han Guo compound sweetener are the same as those of sucrose, low-calorie, and pure natural.
  • the compound sweetener provided by the present invention significantly improves the sweetness performance of the Luo Han Guo extract, especially Mogroside V: the sweetness duration of the Luo Han Guo extract is reduced from 25 to 45 seconds to less than 10 seconds .
  • the method and preparation process of the present invention solve the technical problem that the erythritol compound sweetener is easy to harden. Although erythritol is not easy to absorb moisture and is easy to crystallize, it is generally easy to harden when it is added to the Luo Han Guo extract as a compound sweetener. The combined finished product preparation process solves this problem.
  • the preparation process of the present invention adopts two kinds of processing methods of a kind of raw material for okra: that is, the mucilage of okra young fruit is extracted and separated first under normal temperature and low temperature conditions, the whole process is not heated, and the stability and excellent performance of the mucus are maintained. , reduce the loss of clear flavor; then the obtained extraction residue is subjected to baking and aromatizing treatment, which not only increases the original clear flavor, but also enhances the coke flavor.
  • Raw material utilization is, the mucilage of okra young fruit is extracted and separated first under normal temperature and low temperature conditions, the whole process is not heated, and the stability and excellent performance of the mucus are maintained. , reduce the loss of clear flavor; then the obtained extraction residue is subjected to baking and aromatizing treatment, which not only increases the original clear flavor, but also enhances the coke flavor.
  • the young okra fruit used in the examples of the present invention was purchased from Yongzhou, Hunan, with dark green to light green on the surface, white on the inside, seed particle size of less than 2 mm, and soft texture; Luo Han Guo extract, from Hunan Huacheng Biological Resources Co., Ltd.
  • the company produces (respectively three specifications of Monk fruit powder, V25-35 Mogroside, V50 Mogroside); erythritol, purchased from Baolingbao Biological Co., Ltd.; the purified water used is the second grade pure water used in the production workshop
  • the preparation of water equipment, the chemical reagents and raw and auxiliary materials used are obtained through conventional commercial channels unless otherwise specified.
  • the sweetness duration is determined by sensory measurement; the sweetness multiple is determined by sensory measurement based on sucrose.
  • 1Extraction Take 100kg of young okra, crush it into long strips with a width of about 5mm with a medicine cutter, put it into a 1m3 stirring tank, use water as a solvent, and stir and extract at room temperature of 17°C. 2 times of extraction, 600L of water was added for the first time, and the extraction was performed for 2.0h; After each extraction and filtration, the first extraction residue is then subjected to the second extraction. The 1st and 2nd extracts were combined to obtain 1100L water extract; the extraction residue after the 2nd extraction was collected in another device.
  • 2Clarification First pass the water extract through a disc centrifuge, and then through a complete set of ceramic membrane equipment with a pore size of 500nm for clarification. After feeding the feed liquid, add 300L purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and the washing liquid to obtain 1300L of the ceramic membrane clear liquid.
  • Flavor enhancement Bake the slag obtained from the preparation of okra mucilage according to the following method, first bake it at a temperature of 72°C to a water content of 51%, then bake it at a temperature of 105°C to a water content of 23%, and finally bake it at a temperature of 135°C Roast until a rich burnt aroma is emitted, and 7.9kg of flavor residue is obtained.
  • 3Clarification Clarify the extract through a complete set of ceramic membrane equipment with a pore size of 500 nm. After feeding the feed liquid, add 25L purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and the washing liquid to obtain 85L of the ceramic membrane clear liquid.
  • Decolorization Decolorize the ceramic membrane clear liquid through a complete set of ultrafiltration membrane equipment with a molecular weight cut-off of 10KD. After feeding the material, add 25L purified water to wash the membrane, and concentrate the upstream liquid to 6% solid content to obtain 35L membrane decolorization solution;
  • 2Dissolution Add 90L of purified water to the mixture under constant stirring, and after the solid is completely dissolved, place it in a 5°C freezer and refrigerate until the temperature of the mixed solution is 7°C to obtain a dissolved solution.
  • 3Clarification keep the temperature of the dissolved solution at 7°C and the ambient temperature at 8°C, clarify the dissolved solution through a complete set of ceramic membrane equipment with a pore size of 50nm. After feeding the material, add 25L of purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and water wash liquid to obtain 120kg of ceramic membrane clear liquid.
  • 4Crystallization Concentrate 120kg of ceramic membrane clear liquid under vacuum to 35.2% solid content to obtain 33.0kg of concentrated solution. Then, it was cooled to room temperature and left standing for 4 hours, and a large number of white crystals were precipitated; then the entire crystallization system was placed at 2°C to continue crystallization, and allowed to stand for 5 hours until the crystals were completely precipitated. Suction filtration to collect crystals and mother liquor respectively.
  • Boiling granulation 1Dry the crystals to a water content of 13% to obtain 7.9kg, put into the fluidized bed, keep the boiling state and medium-high wind speed, and the temperature is 72°C; 2The mother liquor is sprayed at a uniform speed of 25kg per hour; 3Mix evenly, to obtain crystalline particles.
  • 1Extraction Take 100kg of young okra, crush it into long strips with a width of about 7mm with a medicine cutter, put it into a 1m3 stirring tank, use water as a solvent, and stir and extract at room temperature of 26°C. 2 times of extraction, 600L of water was added for the first time, and the extraction was performed for 2.0h; After each extraction and filtration, the first extraction residue is then subjected to the second extraction. The 1st and 2nd extracts were combined to obtain 1100L water extract; the extraction residue after the 2nd extraction was collected in another device.
  • 2Clarification First pass the water extract through a disc centrifuge, and then through a complete set of ceramic membrane equipment with a pore size of 300nm to clarify. After feeding the feed liquid, add 300L purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and the washing liquid to obtain 1300L of the ceramic membrane clear liquid.
  • 3Concentration Concentrate the ceramic membrane clear liquid to 4.1% solid content through the complete set of reverse osmosis membrane equipment to obtain 65.8kg milky white okra young fruit mucus.
  • 3Clarification Clarify the extract through a complete set of ceramic membrane equipment with a pore size of 300 nm. After feeding the feed liquid, add 25L purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and the washing liquid to obtain 85L of the ceramic membrane clear liquid.
  • Decolorization Decolorize the ceramic membrane supernatant through a complete set of ultrafiltration membrane equipment with a molecular weight cut-off of 30KD. After feeding the material, add 25L of purified water to wash the membrane, and concentrate the upstream liquid to 8% solid content to obtain 27L of membrane decolorizing solution;
  • the membrane decolorizing solution is concentrated in a short-term vacuum to completely recover ethanol, and concentrate to 25% solid content to obtain 8.6 kg of decolorized okra concentrate juice.
  • 2Dissolution Add 107L of purified water to the mixture under constant stirring, and after the solid is completely dissolved, place it in a 3°C refrigerator and refrigerate until the temperature of the mixed solution is 6°C to obtain a dissolved solution.
  • 3Clarification keep the temperature of the dissolved solution at 6 °C and the ambient temperature at 8 °C, and clarify the dissolved solution through a complete set of ceramic membrane equipment with a pore size of 200 nm. After feeding the material, add 25L of purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and water washing liquid to obtain 147kg of ceramic membrane clear liquid.
  • 4Crystallization Concentrate 147kg of ceramic membrane clear liquid under reduced pressure to 36.5% solid content to obtain 32.8kg of concentrated solution. Then, it was cooled to room temperature and left standing for 6 hours, and a large number of white crystals were precipitated; then the entire crystallization system was placed at 1 °C to continue crystallization, and allowed to stand for 5 hours until the crystals were completely precipitated. Suction filtration to collect crystals and mother liquor respectively.
  • Boiling granulation 1Dry the crystals to a water content of 8% to obtain 9.1kg, put into a fluidized bed, keep the boiling state and medium-high wind speed, and the temperature is 78°C; 2Spray the mother liquor at a uniform speed of 29kg per hour; 3Mix evenly, to obtain crystalline particles.
  • 1Extraction Take 100kg of okra young fruit, crush it into long strips with a width of about 4mm with a medicine cutter, put it into a 1m3 stirring tank, use water as a solvent, and stir and extract at room temperature of 8°C. 2 times of extraction, 600L of water was added for the first time, and the extraction was performed for 2.0h; After each extraction and filtration, the first extraction residue is then subjected to the second extraction. The 1st and 2nd extracts were combined to obtain 1100L water extract; the extraction residue after the 2nd extraction was collected in another device.
  • 2Clarification First pass the water extract through a disc centrifuge, and then through a complete set of ceramic membrane equipment with a pore size of 500nm for clarification. After feeding the feed liquid, add 300L purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and the washing liquid to obtain 1300L of the ceramic membrane clear liquid.
  • 3Clarification Clarify the extract through a complete set of ceramic membrane equipment with a pore size of 500 nm. After feeding the feed liquid, add 25L purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and the washing liquid to obtain 85L of the ceramic membrane clear liquid.
  • 4Decolorization Decolorize the ceramic membrane clear liquid through a complete set of ultrafiltration membrane equipment with a molecular weight cut-off of 10KD. After feeding the material, add 25L purified water to wash the membrane, and concentrate the upstream liquid to 7% solid content to obtain 29L membrane decolorization solution;
  • 2Dissolution Add 211L of purified water to the mixture under constant stirring, and after the solid is completely dissolved, place it in a 5°C freezer and refrigerate until the temperature of the mixed solution is 9°C to obtain a dissolved solution.
  • 3Clarification Keep the temperature of the dissolved solution at 9°C and the ambient temperature at 8°C, and clarify the dissolved solution through a complete set of ceramic membrane equipment with a pore size of 200 nm. After feeding the material, add 25L of purified water to wash the upstream liquid of the ceramic membrane, and combine the effluent and water wash liquid to obtain 253kg of ceramic membrane clear liquid.
  • 4Crystallization Concentrate 253kg of ceramic membrane supernatant under vacuum to a solid content of 37.6% to obtain 52.9kg of concentrated solution. Then, it was cooled to room temperature and stood for 5 hours, and a large number of white crystals were precipitated; then the entire crystallization system was placed at 2°C to continue crystallization, and allowed to stand for 6 hours until the crystals were completely precipitated. Suction filtration to collect crystals and mother liquor respectively.
  • Boiling granulation 1Dry the crystals to a water content of 11% to obtain 16.1kg, put into a fluidized bed, keep the boiling state and medium-high wind speed, and the temperature is 76°C; 2Spray the mother liquor at a uniform speed of 21kg per hour; 3Mix evenly, to obtain crystalline particles.
  • Example 3 Others are the same as Example 3, except that the consumption of okra young fruit mucilage is 25 parts, and the consumption of okra concentrated juice is 50 parts.
  • Example 3 Others are the same as Example 3, the difference is that in the preparation of okra concentrated juice in step (2), the extraction residue is directly baked at a temperature of 135°C until it emits a burnt aroma, that is, the baking at a temperature of 67°C and a temperature of 106°C is not performed.
  • step (2) preparing the concentrated okra juice
  • step (3) preparing the concentrated okra juice
  • step (2) preparing the concentrated okra juice
  • step (3) increasing the fragrance: the extraction residue obtained from the mucilage of young okra fruit is baked according to the following method, and first baked at a temperature of 70 ° C to a water content 45%, then bake at a temperature of 106°C to a water content of 26%, and finally bake at a temperature of 120°C.
  • step (2) preparing the concentrated okra juice
  • step (3) preparing the concentrated okra juice
  • 1. increasing the fragrance the extraction residue obtained from the mucilage of young okra fruit is baked according to the following method, and first baked at a temperature of 70 ° C to a water content 45%, then bake at a temperature of 106°C to a water content of 26%, and finally bake at a temperature of 150°C, the obtained flavor residue has a slightly burnt taste.
  • step (3) mixing, dissolving and clarifying: 5 Boiling granulation: 1 Dry the crystals to a water content of 17%. The final product is placed in the air for a period of time, and there is a problem of partial hardening.
  • step (3) Others are the same as in Example 3, except that in step (3), 1. in mixing, okra young fruit mucilage is not added, and the consumption of okra juice concentrate is 75 parts simultaneously.
  • step (3) 1. in mixing, okra juice concentrate is not added, and the consumption of okra young fruit mucilage is 75 parts simultaneously.
  • the compound sweeteners obtained in the above examples and comparative examples are prepared into an aqueous solution with mineral water, and the dilution ratio is such that the sweetness of the diluted aqueous solution is close to that of the 5% sucrose aqueous solution, that is, the sweetness is close to 1. After that, the following tests were carried out, and the results are listed in Table 1:
  • the sensory assessors were screened. After the taste sensitivity training, 20 sensory assessors (half male and half) were finally screened to form a sensory assessment team.
  • Duration of sweetness Please taste the compound sweetener aqueous solution diluted to a sweetness close to 5wt% sucrose solution, and take 5wt% sucrose solution as the control group, and record the test from the time the assessor drinks it. The time at which the sweetness disappeared, excluding those who tasted the 5 wt% sucrose solution with a sweetness duration of more than 1 second, i.e., those who tasted the 5 wt% sucrose solution with a sweetness duration of less than 4 seconds and Data for subjects greater than 6 seconds. The final average obtained is the sweetness duration of the compound sweetener of the present invention.
  • the test samples are divided into a compound group and a control group, the compound group is the compound composition product obtained according to the formula in the embodiment, and the control group is a 5wt% sucrose solution.
  • the assessor held it in the mouth, stayed for a few seconds, and spit it out.
  • the assessment time interval was 20 minutes.
  • the assessment result was the average of the scores of the 10 assessors.
  • the sensory evaluation standard of the control group was 10 points out of 10.
  • the compaction of the compounded sweeteners was tested: the compounded sweeteners obtained in the examples and comparative examples were stored at 25°C and 65RH% for 24 hours, and the moisture absorption rate and the compaction were tested.
  • commercially available sucrose was used as the test substance.
  • the present invention utilizes two kinds of raw materials from okra, that is, okra mucilage and okra young fruit mucilage extraction residue are baked and extracted to obtain okra concentrated juice, and Luo Han Guo extract, after erythritol is compounded
  • the obtained compound sweetener can effectively shorten the sweetness duration of the Luo Han Guo extract, that is, improve the after-sweetness problem of the Luo Han Guo-based sweetener, thereby broadening the Luo Han Guo extract as a sweet compound agent
  • the use in improves the economic value of Luo Han Guo.
  • the compound sweetener obtained by the present invention not only solves the problem of post-sweetness of the Luo Han Guo extract, but also enables the compound sweetener to have a special fruit aroma through a specific baking process, thereby improving the taste of the sweetener .

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Abstract

一种改善罗汉果提取物持久甜味和甜度倍数的复配甜味剂，采用的原料包括：秋葵幼果粘液，秋葵浓缩汁，罗汉果提取物、赤藓糖醇，其中罗汉果提取物中罗汉果甜苷V的质量为秋葵幼果粘液和秋葵浓缩汁总质量的0.3-1%。该复配甜味剂通过秋葵幼果粘液增加稠厚口感，通过烘培脱色的秋葵浓缩汁增加甜味饱和度，使甜味时间小于10秒，改善了罗汉果提取物的持久甜味。同时，该复配甜味剂苦涩度口感、甜味持续时间接近蔗糖，是一种可以替代蔗糖的低热量、纯天然甜味剂。

Description

一种改善罗汉果提取物持久甜味的复配甜味剂及其制备方法 技术领域
本发明涉及植物提取分离技术领域及甜味剂复配领域，具体涉及一种改善罗汉果提取物持久甜味的复配甜味剂及其制备方法。
背景技术
罗汉果提取物是以葫芦科植物罗汉果的新鲜成熟果实为原料，先糖化后熟，再经一系列分离提取步骤制备而得。罗汉果提取物是所有天然甜味物质中口感最好、最接近蔗糖的品种，具有蔗糖的清爽甜味、高甜度、低热量的显著优点，不改变血压和血糖、不引起龋齿，特别适用于糖尿病、高血压、肥胖以及不宜食糖人群，也是健康人群的理想代糖品，无甜菊糖苷的后苦味和金属味，也无甜茶苷的先苦后甜口感，因此，最容易被所有人群接受，这是显著优点；但其主要缺点在于甜味持久，以及甜度倍数高而限制了直接使用。
蔗糖的甜味口感是入口即感到甜味，约1-2秒达到甜度峰值，约5秒消失，这是目前最理想的甜味口感。但是目前不管是合成的，还是天然的高倍甜味剂问题是后甜味太重，影响口感。
罗汉果提取物主要包括：(1)罗汉果粉，其制备工艺主要包括破碎、提取、过滤、浓缩、干燥等，其中罗汉果苷V含量为0.5～4％；(2)V25～35罗汉果甜苷，其制备工艺主要包括破碎、提取、过滤、澄清、层析、浓缩、干燥等步骤，其中罗汉果苷V含量为25～35％；(3)V50罗汉果甜苷，其制备工艺主要包括破碎、提取、过滤、澄清、层析、脱色、脱盐、浓缩、干燥等步骤，其中罗汉果苷V含量为50～60％；(4)罗汉果浓缩汁，其制备工艺主要包括破碎、提取、过滤、澄清、脱色、脱盐、浓缩等步骤，其中罗汉果苷V含量为0.5～5％。
由于罗汉果浓缩汁以液体形式存在，极难干燥，不易储存，本发明并不涉及，在此主要涉及固体形式存在的罗汉果提取物。
罗汉果提取物均具有一定缺陷：(1)罗汉果粉、V25～35罗汉果甜苷：1％水溶液呈浑浊状态，或具有明显的后沉淀现象，限制了在饮料等对澄清度有要求的终端产品中的应用；(2)罗汉果粉：未经分离提纯，保留了原存于鲜罗汉果中的大部分物质，虽 然甜味接近饱和，但无稠厚口感，仍具有持久甜味，只是比高含量罗汉果甜苷的时间短，其甜味持续时间约25秒；甜度略高，为蔗糖的14倍左右；(3)V25～35罗汉果甜苷：经分离提纯，去除了原存于鲜罗汉果中的大部分物质，导致甜味不饱和，也无稠厚口感，具有明显的持久甜味，其甜味持续时间约45秒；甜度高，为蔗糖的100倍左右；(4)V50罗汉果甜苷：经分离提纯，去除了原存于鲜罗汉果中的大部分物质，导致甜味不饱和，也无稠厚口感，具有明显的持久甜味，其甜味持续时间约45秒；甜度高，为蔗糖的200倍左右。
罗汉果提取物中罗汉果甜苷V是一种理想的高倍天然甜味剂，但是由于其后甜味比较严重，制约了其在各种甜味剂中的作用。
秋葵，又名羊角豆、咖啡黄葵、毛茄，为锦葵科植物咖啡黄葵的幼果，它的可食用部分是果荚，又分绿色和红色两种；其脆嫩多汁，滑润不腻，香味独特，被许多人所喜爱；具有利咽，通淋，下乳，调经之功效；常用于咽喉肿痛，小便淋涩，产后乳汁稀少，***。
秋葵的成分主要有：
1、粘液。
秋葵有特殊的黏液，在花后5d的嫩果中黏度最高，黏液是秋葵品质的重要评价指标，主要成分是糖类化合物，包括果胶、聚多糖和糖蛋白等物质。
秋葵果胶在嫩果荚中含量最高，嫩果种子、成熟果荚次之，分别为20.97％、9.34％、8.91％；在不同品系中嫩果荚中最高24.05％，最低15.69％。秋葵果胶至少有9种单糖组成，主要是半乳糖醛酸、半乳糖、鼠李糖、葡萄糖；以RG-I型结构为主，糖醛酸41.43％，甲酯化度49.86％，pH＝4.63，溶解度82％，属弱酸性低酯果胶；热稳定性好，黏度与其质量浓度正相关，与加热温度、时间负相关。
2、蛋白质和氨基酸
秋葵蛋白质含量较多，鲜嫩果实2.3％，成熟果实3.15％，种子28.1％；氨基酸种类齐全，目前已分离鉴定出17种。
3、维生素和微量元素
秋葵含有丰富的V C、B族和V A、V E、V K，每100克秋葵鲜嫩果实中，含有V A 198μg、V B1 0.2mg、V B2 0.06mg、V C 44mg、V E 1.03mg，V C和V E含量较多。
秋葵中矿质元素丰富，含有微量元素13种，按照测定的最高含量(mg/100g)，分别为K 95、Ca 343、P 65、Mg79.36、Mn 56.4、Zn 38.9、Cu 26.2、Se 11、Fe 2.71、Cr 0.410、Pb 0.745、Cd 0.319。
4、黄酮
秋葵含有丰富的黄酮及酚酸类化合物，果实中黄酮总量2.8％，目前已分离鉴定了12个黄酮成分，分别为槲皮素-3-O-二葡萄糖苷、杨梅黄素-3-O-葡萄糖苷、槲皮素-3-O-葡萄糖-木糖苷、槲皮素-3-O-芸香糖苷、槲皮素-3-O-葡萄糖苷、异鼠李亭-3-O-葡萄糖-戊糖苷、槲皮素-3-O-(丙二酰基)葡萄糖苷、杨梅黄素-3-O-鼠李糖苷、4，5，7-三羟基黄酮-O-葡萄糖苷、杨梅黄素、4，5，7-三羟基黄酮和槲皮素。
目前国内对罗汉果提取物的研究很多，对加入罗汉果甜苷的复配甜味剂的研究也很多，有大量文献和专利报导，但其主要从两方面展开：一是加入苦味剂来改变罗汉果甜苷的甜味持续时间；二是加入赤藓糖醇以及多种物质复配并以简单工艺制备。另外，所用罗汉果提取物主要为罗汉果甜苷，且主要为罗汉果苷V含量50％以上的罗汉果甜苷，未涉及罗汉果粉等只有较低含量罗汉果苷V的罗汉果提取物，尚无通过特殊的植物提取物来改变罗汉果提取物的甜味持续时间和甜度倍数的报道。
现有技术中有将罗汉果和秋葵的成分在一起配制为茶饮料的方法，但是还没有现有技术披露采用秋葵成分和罗汉果提取物复配制备甜味剂的方法。
现有公开的有关改变罗汉果甜苷甜味时间和以罗汉果甜苷为主的复配甜味剂的技术内容及解决方案如下：
1、加入苦味剂以改变罗汉果甜苷的甜味时间
例如，CN201610005411.9公开了一种改变罗汉果甜苷甜味时间轮廓的甜味剂及其制备方法，但是该专利的效果并不理想。本发明人通过实验证明，加入芦丁并未能使罗汉果甜苷水溶液的入口甜度增加，反而增加了苦味口感；在缩短甜味时间的同时，也增强了苦味口感，且缩短时间越短，苦味越明显，导致其口感无法接受。另外，该专利并未改变罗汉果甜苷的甜度倍数。
2、以罗汉果甜苷为主的复配甜味剂
例如，CN201910902694.0公开了一种平抑血糖的罗汉果复配甜味剂及其制备方法；CN201810374254.8公开了一种含有罗汉果甜苷的低糖分焦糖风味组合物、制备方法和 应用；CN201810374974.4公开了一种罗汉果甜苷复配组合物及其应用；；CN201710035875.9公开了一种两倍糖或多倍糖的健康型罗汉果糖的制作方法，属于食品技术领域；CN201410365736.9公开了一种具有低血糖指数的罗汉果饮料；CN200510055228.1公开了一种添加了罗汉果提取物的甜味剂及其制备方法；CN200410022754.3公开一种低热量罗汉果糖；CN201911372029.1公开了一种天然复配甜味剂及其制备方法；CN201910548599.5公开了一种复配甜味剂的生产方法，涉及食品添加剂生产技术领域；CN201910322941.X公开了一种低热量复配甜味剂及其制备方法；CN201310616422.7公开了一种天然复配甜味剂及其制备方法。
上述有关罗汉果复配甜味剂的发明均是在罗汉果提取物的基础上加入一种或多种甜味剂，如甜菊糖苷、阿洛酮糖、三氯蔗糖等；包含物质种类多，如糖醇类、甘露糖等，无法突出一些物料的优异性能；并以简单工艺，如混合、干燥，或制粒、干燥等制备而得，内外难以实现成分均一。普遍存在成分复杂，效果不明显，一些物料的缺陷明显的问题。以上关于改变罗汉果甜苷甜味持续时间和罗汉果甜苷为主的复配甜味剂，方法及效果不甚理想，具体表现在：(1)加入苦味剂来改变罗汉果甜苷甜味时间的方法及其复配甜味剂，至今未有企业采用类似方法及相关甜味剂面世。主要原因是苦味剂的加入改变了罗汉果甜苷的清爽甜味口感，未对罗汉果提取物的持久甜味产生明显影响，未增加入口甜味，反而引入了苦味，导致口感无法接受；(2)罗汉果复配甜味剂处方复杂，加入多种物质，使得罗汉果甜苷侧重于功能性，偏向于功能性食品，并不是所有人群适用，离作为单一甜味剂使用的目标有差距；(3)包含糖醇种类多，均具有明显副作用并有使用限量，且组合性能欠缺；(4)加入树胶类来增加稠厚口感，即加入食品添加剂，且单一加入，不仅改变甜味时间的效果难以保证，而且添加物也不易被接受；(5)风味欠缺。罗汉果复配甜味剂缺乏特殊的清香味，而往往复配的甜味剂组合物会缺失这部分香味和稠厚口感、甜味饱和度；(6)制备工艺简单，加上配方中添加物的原因，导致目前市场上的罗汉果复配甜味剂普遍存在易板结的难题，现有的解决方法主要通过往包装袋内充入惰性气体来阻止含赤藓糖醇的罗汉果复配甜味剂板结，尚未从成分角度根本上解决板结难题，使得用户在使用过程中不可避免遇到板结而影响使用，品质有待提升。以上现有技术都没有有效改善罗汉果甜苷V的后甜味问题。
发明内容
本发明所要解决的技术问题是，克服现有技术中基于罗汉果提取物，特别是罗汉果 甜苷V后甜味较重影响口感的问题，扩大作为天然高甜度甜味物质的罗汉果提取物的应用范围。以罗汉果提取物中的罗汉果粉、V25～35罗汉果甜苷、V50罗汉果甜苷作为高甜物质；以秋葵的提取物作为改良口感的物质，和罗汉果提取物复配后产生了协同配合的作用，不仅能缩短罗汉果甜苷V的甜味持续时间，经过特定的烘焙程序，还为复配的甜味剂带来特殊的香味。本发明提供的改善罗汉果提取物持久甜味的复配甜味剂，从气味、稠厚口感、甜味饱和度三方面得到了综合口感最佳的产品，使所得罗汉果复配甜味剂的甜味持续时间小于10秒。本发明提供的罗汉果复配甜味剂，其滋味口感、甜味持续时间同蔗糖、低热量、纯天然，具有特殊的宜人的果蔬清香味，可作为各种人群的理想代糖产品。本申请的发明人经过大量实验对比发现，在和5％蔗糖溶液甜度接近的情况下，本发明的甜味剂溶液的甜味在10秒内消失，均可作为理想的甜味剂。
本发明解决其技术问题所采用的技术方案如下：一种改善罗汉果提取物持久甜味和甜度倍数的复配甜味剂，包括原料：秋葵幼果粘液，秋葵浓缩汁，罗汉果提取物、赤藓糖醇，条件是罗汉果提取物中罗汉果甜苷V的质量为秋葵幼果粘液和秋葵浓缩汁总质量的0.3-1％。
进一步地，所述复配甜味剂把包括以下质量份的原料：30-50份秋葵幼果粘液，15-25份秋葵浓缩汁，1-30份罗汉果提取物、100-500份赤藓糖醇。
优选地，罗汉果提取物中罗汉果甜苷V的质量为秋葵幼果粘液和秋葵浓缩汁总质量的0.5-0.8％。
赤藓糖醇在100-500份较宽的范围可调，目的是根据需求得到不同甜度的甜味剂产品，条件是复配甜味剂的甜度不超过蔗糖的十倍。更为理想的，复配甜味剂的甜度是蔗糖的1-6倍。
优选地，秋葵幼果粘液中固形物的含量为2-10％，优选4-7％；秋葵浓缩汁中固形物的含量为20-30％。
本发明所用到的秋葵幼果粘液是通过包括以下步骤的制备方法得到：秋葵幼果用水提取，收集提取渣和提取液，提取液过滤后浓缩得到秋葵粘液。
在秋葵粘液的制备方法中有以下优先的技术方案：
进一步地，所述秋葵幼果为花谢后4～7天即采收，其标准为：首先要保证果荚坚韧、色泽明亮、膨大且未老化。秋葵的采收标准会随着温度的变化而有所不用，在高温时，秋葵果荚的长度大约在10厘米左右，而温度较低时，长度大约只有8厘米。果荚 的长度都要保持在10厘米以内。只有秋葵幼果才含有丰富的粘液，并具有特殊的果蔬清香味。随着果子成熟，粘液含量急剧下降，而熟透的秋葵已无法嚼动。
进一步地，提取的温度是8-30℃，优选8-15℃。维持较低的提取温度的优点在于保持秋葵浓缩汁的原生态果蔬清香味和稠厚口感的优良性能，保持秋葵粘液胶体溶液的稳定性，防止高温破坏胶体溶液的稳定性和增色。
进一步地，提取所用水的质量是秋葵幼果质量的8-15倍，优选多次提取，比如两次，三次，四次进行提取，每次提取用水的量依次递减，递减的量不超过上次用水提取的20％。
进一步地，所述过滤和浓缩没有特别的限定，本领域常规过滤和浓缩方法即可，比如过滤是陶瓷膜过滤，陶瓷膜材质为氧化铝或者氧化锆，孔径是300-500nm；浓缩是反渗透膜浓缩，浓缩至固形物含量为1-5％即可。因为秋葵幼果粘液具有一定的粘稠度，过浓可能导致反渗透膜的浓缩效果。
本发明所用到的秋葵浓缩液是通过包括以下步骤的制备方法得到：取秋葵幼果粘液制备过程中的提取渣，进行烘焙后得到风味渣，风味渣用醇水溶液提取，经过过滤，脱色，浓缩得到秋葵浓缩液。
在秋葵浓缩液的制备方法中有以下优选的技术方案：
进一步地，所述烘焙是在130-140℃下进行烘焙出焦香味，烘焙时间为0.5-1.5h。发明人发现，在上述温度范围内进行烘焙，提取渣发生了一系列复杂的化学变化，能够产生浓郁的焦香味，采用这种烘焙后的风味渣提取得到浓缩液和罗汉果提取液复配后，不仅能缩短复配甜味剂的甜味时间，明显改善罗汉果提取物复配的甜味剂的后甜味严重的问题，而且还能带来特殊的果香味。
优选地，在进行烘焙前，先在较低温度下进行脱水的处理，即在65-100℃下将提取渣的含量水降低到30％以下。更优选地，所述脱水处理，是提取渣先在60-70℃下烘烤0.5-1h，使含水量在50％以下，再在90-100℃下烘烤0.5-1h，使含水量在30％以下。通过预处理和烘焙处理的增香，可显著增加秋葵的果蔬清香味和焦香味，秋葵幼果粘液协同从气味方面辅助改善罗汉果提取物的持久甜味和口感。
所述醇水溶液中，醇的体积浓度为60-80％，优选为乙醇的水溶液。
所述过滤，脱色，以及浓缩的步骤是本领域所熟知的，优选地，所述过滤是通过陶瓷膜得澄清液；所述脱色是通过超滤膜，截留分子量为8KD～30KD，超滤也起到一定 的浓缩作用，浓缩至固形物含量5-10％；所述浓缩是真空浓缩，浓缩至固形物含量20-30％。采用真空浓缩的好处是可以减少秋葵果蔬清香味和焦香味的损失。
所述罗汉果提取物可以按照提取物中罗汉果甜苷V的含量，分为不同的规格，从商品可购买的角度，一般可以分为(1)罗汉果粉(罗汉果苷V含量0.5～4％)；(2)V25～35罗汉果甜苷(罗汉果苷V含量25～35％)；(3)V50罗汉果甜苷(罗汉果苷V含量50～60％)。
罗汉果提取物的加入量需要满足罗汉果提取物中罗汉果甜苷V的质量是秋葵幼果粘液和秋葵浓缩汁总质量的0.3-1％，优选地，罗汉果提取物中罗汉果甜苷V的质量是秋葵幼果粘液和秋葵浓缩汁总质量的0.5-0.8％。
发明人预料不到地发现，以秋葵幼果粘液和秋葵粘液提取渣经过烘焙处理后的提取浓缩液和罗汉果提取物一起复配，在罗汉果提取物中主要甜味物质的罗汉果苷V的质量占秋葵幼果粘液和秋葵浓缩汁总质量的一定含量内，能够有效缩短罗汉果甜苷V的后甜味，解决罗汉果提取物作为高倍甜味剂的后甜问题，而且复配后的甜味剂具有特殊的果香味，口感很好。而且本发明提供的甜味复配剂主要复配的辅料来源于秋葵，价廉易得，是极具市场竞争力的复配甜味剂产品。
本发明还提供了所述改善罗汉果提取物持久甜味和甜度倍数的复配甜味剂的制备方法，包括以下步骤：将秋葵粘液、秋葵脱色风味浓缩汁、罗汉果提取物、赤藓糖醇按一定比例混合，溶解，过滤，结晶，沸腾制粒，干燥即得。
优选地，在沸腾制粒前，对结晶所得晶体进行干燥至含水量＜15％。
作为本发明复配甜味剂制备方法优选的技术方案：
进一步地，所述溶解的温度是5-15℃，水的体积加入量为赤藓糖醇重量的2～15倍(V/W)。优选采用较低的温度溶解，目的是使混合溶液体系的沉淀和后沉淀析出尽可能完全，而赤藓糖醇不析出，有利于去除沉淀和后沉淀。采用此规格陶瓷膜，可以将溶液体系的沉淀和后沉淀完全去除，得到在低温和常温条件下均无沉淀和后沉淀的溶液。
进一步地，所述过滤，是采用陶瓷膜，材质为氧化铝或氧化锆，陶瓷膜的孔径为50-200nm。
进一步地，所述结晶，可以采用一步结晶或者分步结晶，优选采用分步结晶方式。具体是先将陶瓷膜清液浓缩至固形物含量30～40％，然后在室温条件下析出均匀的混合物结晶；低温是1～4℃，即在常温析出结晶的基础上进一步析出均匀的混合物结晶。此 结晶方法可以得到混合均匀、内外完全一致、具有结晶光泽的混合物结晶。
进一步地，在沸腾制粒之前，对得到的结晶先干燥至含水量≤15％，干燥的方式是本领域所熟知的，比如真空干燥，鼓风干燥。所述沸腾制粒，是以结晶所得晶体为载体，所得结晶母液为喷入液。采用沸腾制粒法可以避免了外加粘合剂或水，保持了原结晶形态，并使结晶母液与结晶得到充分、完全的混合均匀，且结晶母液主要在外层，其中的赤藓糖醇与其他物质相结合，防止的后期干燥的结晶颗粒板结。所述结晶载体要求先干燥至含水量≤15％。这样可以避免产品在空气中的板结问题，如果水分过高，易在受热过程中发生晶形溶解与变化，导致晶形不统一；而且也会导致产品的板结。
若结晶过于潮湿，则易在受热过程中发生晶形溶解与变化，导致晶形不统一，影响外观及产品质量。
所述干燥，温度为55～65℃；干燥方式为鼓风干燥，或真空干燥，或微波真空干燥，或带式真空干燥，真空度小于-0.085MPa。
本发明的技术思路如下,分别从制备工艺和产品的口感进行解释：
1、制备工艺
秋葵含有丰富的粘液，即使在较低温度下，也可以溶于水中，因此，控制适当的加水量以及提取次数，可以将这些成分完全提取出来，并保留秋葵所特有的果蔬清香味。若温度过高，则这些成分容易被破坏，并形成不稳定的胶体溶液，从而破坏了溶液稳定性，导致粘液不易分离纯化，以及无法明显增加稠厚口感。通过离心去除大部分机械杂质以后，再通过陶瓷膜的微滤澄清，可以得到澄清的富含粘液的溶液。再通过具有一定截留分子量的超滤膜，实现具有分子空间位阻的色素与具有极大分子量的粘液在常温条件下的分离，从而制备得到秋葵脱色粘液。
秋葵经水提所得提取渣，仍具有一些不被低温水溶液所提取出来的物质，在一定条件下，这些物质经过烘烤，可以散发出浓郁的果蔬清香味以及焦香味，而这种清香味与新鲜秋葵经烘烤所产生的气味一致。因此，先低温提取秋葵粘液，再对提取渣进行增香增味，不仅得到质量好，稳定的粘液，还可以得到秋葵所特有的浓郁的果蔬清香味和焦香味。为了完全提出水提渣中的成分，用一定浓度的含水醇，可以在较低温度下将这些成分提取出来，并不损失香味成分。再经过陶瓷膜的微滤澄清技术去除少量杂质和沉淀，并通过反渗透膜和真空减压浓缩制备得到秋葵风味浓缩汁。
由于罗汉果提取物中的罗汉果粉、V25～35规格溶于水中具有沉淀和后沉淀现象， 因此，在将秋葵脱色粘液、风味浓缩汁和罗汉果提取物、赤藓糖醇混合以后，控制较低的温度和操作条件，在赤藓糖醇不结晶析出的条件下，再通过孔径更小的陶瓷膜过滤去除这些沉淀以及后沉淀，进一步提高了产品的澄清度。通过将液体浓缩至一定体积的情况下，使混合物由于体积下降而结晶析出，再进一步降低体系温度，从而使结晶析出更完全。此种结晶方法使混合物中的结晶大部分析出，并保证了结晶的完好晶形、光泽以及成分均一性。通过干燥控制结晶的含水量，并将结晶作为载体，运用沸腾制粒技术，控制好风速和温度，使结晶与母液再度结合。而母液中仅留存少量物质，再将母液在沸腾制粒过程中定期均匀喷入，从而得到品相好的罗汉果复配甜味剂结晶。同时，由于母液中的主要成分来源于秋葵，具有一定的疏水性，与赤藓糖醇的不易吸潮性质相辅相成，显著改变了赤藓糖醇复配甜味剂的板结时间，使产品使用更方便。
2、改善罗汉果提取物持久甜味和甜度倍数
罗汉果提取物，无论是罗汉果粉，还是V25～35和V50罗汉果甜苷，都存在持久甜味，只是甜味持续时间有些差异，从25秒至45秒不等；它们都是天然高效甜味物质，只是由于罗汉果苷V的含量不同，而使其甜度为蔗糖的15倍至200倍不等。
秋葵幼果含有丰富的粘液，是一种糖聚合体，主要成分为果胶、可溶性膳食纤维、羟甲基纤维素等，使得其溶液具有稠厚口感。另含丰富的蛋白质和氨基酸等成分，并具有特殊的果蔬清香味。这些特殊的成分，使得秋葵粘液及其提取物具有特殊作用：即可以通过增加罗汉果提取物溶液的稠厚口感，提高甜味饱和度，并通过特殊的宜人的气味，协同作用，大大改善罗汉果提取物的持久甜味，并适当降低甜度倍数。
赤藓糖醇具有清爽的甜味口感，作为一种填充型低甜度甜味剂，可以在秋葵的基础上进一步改善罗汉果提取物的持久甜味，并显著降低甜度倍数。赤藓糖醇极易结晶，虽然不吸潮，但主含赤藓糖醇的复配甜味剂容易板结，这是一个难题。而秋葵粘液和秋葵醇提制备所得浓缩汁，在一定程度上可以显著延缓赤藓糖醇的板结时间，使其不易板结，这也是相互作用的结果。
通过低温提取分离的秋葵粘液、增香增味的秋葵醇提浓缩汁，以及赤藓糖醇的协同作用，控制相应的比例，实现了罗汉果提取物的甜味持续时间从45秒缩短至小于10秒，从而制备得到改善了罗汉果提取物持久甜味的复配甜味剂。
本发明的有益效果在于：
(1)本发明提供了一种改善罗汉果提取物持久甜味的复配甜味剂。通过秋葵幼果粘 液增加稠厚口感，经增香工艺及含水醇提取制备的秋葵浓缩汁增加甜味饱合度，与秋葵所特有的果蔬清香味以及经增香工艺所得焦香味，三方面因素协同改善罗汉果提取物的持久甜味；并通过赤藓糖醇的低甜度、清爽口感进一步改善罗汉果提取物的持久甜味，稀释甜度倍数。该罗汉果复配甜味剂的苦涩度口感、甜味持续时间同蔗糖、低热量、纯天然。
(2)本发明提供复配甜味剂显著改善了罗汉果提取物，特别是其中罗汉果甜苷V的甜味性能：使罗汉果提取物的甜味持续时间从25～45秒，降低至10秒以内。
(3)本发明的方法及制备工艺解决了赤藓糖醇复配甜味剂易板结的技术难题。虽然赤藓糖醇不易吸湿、易结晶，但加入到罗汉果提取物中作为复配甜味剂普遍存在易板结的问题，本方法通过秋葵配方及制备工艺的不同，以及结晶和沸腾制粒相结合的成品制备工艺，解决了这一难题。
(4)本发明制备工艺将秋葵采用一种原料两种处理的方式：即先在常温和低温条件下提取分离秋葵幼果粘液，整个过程不加热，保持其粘液的稳定性和优良性能，减少清香味的损失；然后对所得提取渣进行烘烤增香处理，不仅增加了原有清香味，还增强了焦香味，并采用含水醇将水提之后的成分尽可能完全提取出来，提高原料利用率。
具体实施方式
以下结合实施例对本发明进行进一步的说明。
本发明实施例所使用的秋葵幼果，购于湖南永州，表面为深绿至浅绿色，内面白色，种子粒径小于2mm，质地较软；罗汉果提取物，为湖南华诚生物资源股份有限公司生产(分别为罗汉果粉，V25～35罗汉果甜苷，V50罗汉果甜苷三个规格)；赤藓糖醇，购于保龄宝生物股份有限公司；所使用纯化水为生产车间用二级纯水设备制备，所使用的化学试剂和原辅材料，如无特殊说明，均通过常规商业途径获得。
本发明实施例中，甜味持续时间用感观测定；甜度倍数，以蔗糖为基准，感观测定。
实施例1
本实施例包括以下步骤：
(1)制备秋葵幼果粘液：
①提取：取100kg秋葵幼果，用切药机破碎成宽度约5mm的长条形细块，投入1m 3搅拌罐中，以水为溶媒，在室温17℃搅拌提取。提取2次，第1次加水600L，提取2.0h；第2次加水500L，提取1.5h。每次提取完过滤，第1次提取渣再进行第2次提取。合 并第1次和第2次提取液，得1100L水提取液；第2次提取后的提取渣另器收集。
②澄清：先将水提取液过碟式离心机，再过孔径为500nm的陶瓷膜成套设备澄清。进完料液后，加300L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得1300L陶瓷膜清液。
③浓缩：将陶瓷膜清液通过反渗透膜成套设备浓缩至3.6％固形物含量，得72.2kg乳白色的秋葵幼果粘液。
(2)制备秋葵浓缩汁：
①增香：将制备秋葵粘液所得提取渣按以下方法烘烤，先在温度72℃烘烤至含水量51％，再在温度105℃烘烤至含水量23％，最后在温度135℃烘烤至散发出浓郁的焦香味，得7.9kg风味渣。
②提取：将7.9kg风味渣投入100L夹套搅拌罐中，以62％乙醇为溶媒，加热至54℃保温搅拌提取。提取2次，第1次加溶媒50L，提取2.0h；第2次加溶媒40L，提取1.5h。每次提取完过滤，第1次提取渣再进行第2次提取，第2次提取渣经回收乙醇后弃去。合并第1次和第2次提取液，得73L乙醇提取液。
③澄清：将提取液通过孔径为500nm的陶瓷膜成套设备澄清。进完料液后，加25L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得85L陶瓷膜清液。
④脱色：将陶瓷膜清液通过截留分子量为10KD的超滤膜成套设备脱色。进完料以后，加25L纯化水洗膜，并将上游液浓缩至6％固形物含量，得35L膜脱色液；
⑤回收乙醇：将膜脱色液通过短时真空浓缩完全回收乙醇，并浓缩至21％固形物含量，得10kg脱色的秋葵浓缩汁。
(3)混合、溶解、澄清：
①混合：取步骤(1)制备得到的秋葵幼果粘液30份、步骤(2)制备得到的秋葵浓缩汁25份、罗汉果粉(罗汉果苷V含量3.5％)8份、赤藓糖醇100份，混合，得混合物。
②溶解：在不断搅拌下向混合物中加入90L纯化水，待固体完全溶解后，置5℃冷库冷藏至混合溶液温度为7℃，得溶解液。
③澄清：保持溶解液温度为7℃，环境温度8℃操作，将溶解液通过孔径为50nm的陶瓷膜成套设备澄清，进完料以后，加25L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得120kg陶瓷膜清液。
④结晶：将120kg陶瓷膜清液真空减压浓缩至35.2％固形物含量，得33.0kg浓缩液。然后冷却至室温，静置4h，析出大量白色结晶；再将结晶体系整体置2℃继续析晶，静置5h，至结晶析出完全。抽滤，分别收集结晶和母液。
⑤沸腾制粒：①将结晶干燥至含水量13％，得7.9kg，投入流化床，保持沸腾状态和中高风速，温度72℃；②将母液按每小时25kg匀速喷入；③混合均匀，得结晶颗粒。
⑥干燥：控制温度61℃，真空度-0.09MPa，将结晶颗粒真空干燥，得到11.3kg罗汉果复配甜味剂。
实施例2
(1)制备秋葵幼果粘液：
①提取：取100kg秋葵幼果，用切药机破碎成宽度约7mm的长条形细块，投入1m 3搅拌罐中，以水为溶媒，在室温26℃搅拌提取。提取2次，第1次加水600L，提取2.0h；第2次加水500L，提取1.5h。每次提取完过滤，第1次提取渣再进行第2次提取。合并第1次和第2次提取液，得1100L水提取液；第2次提取后的提取渣另器收集。
②澄清：先将水提取液过碟式离心机，再过孔径为300nm的陶瓷膜成套设备澄清。进完料液后，加300L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得1300L陶瓷膜清液。
③浓缩：将陶瓷膜清液通过反渗透膜成套设备浓缩至4.1％固形物含量，得65.8kg乳白色的秋葵幼果粘液。
(2)制备秋葵浓缩汁：
①增香：将制备秋葵幼果粘液所得提取渣按以下方法烘烤，先在温度70℃烘烤至含水量47％，再在温度95℃烘烤至含水量26％，最后在温度140℃烘烤至散发出浓郁的焦香味，得7.8kg风味渣。
②提取：将7.8kg风味渣投入100L夹套搅拌罐中，以68％乙醇为溶媒，加热至56℃保温搅拌提取。提取2次，第1次加溶媒50L，提取2.0h；第2次加溶媒40L，提取1.5h。每次提取完过滤，第1次提取渣再进行第2次提取，第2次提取渣经回收乙醇后弃去。合并第1次和第2次提取液，得73L乙醇提取液。
③澄清：将提取液通过孔径为300nm的陶瓷膜成套设备澄清。进完料液后，加25L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得85L陶瓷膜清液。
④脱色：将陶瓷膜清液通过截留分子量为30KD的超滤膜成套设备脱色。进完料以 后，加25L纯化水洗膜，并将上游液浓缩至8％固形物含量，得27L膜脱色液；
⑤回收乙醇：将膜脱色液通过短时真空浓缩完全回收乙醇，并浓缩至25％固形物含量，得8.6kg脱色的秋葵浓缩汁。
(3)混合、溶解、澄清：
①混合：取步骤(1)的得到的秋葵幼果粘液25份、步骤(2)的得到的秋葵浓缩汁15份、V25～35罗汉果甜苷(罗汉果苷V含量33.6％)0.9份、赤藓糖醇300份，混合，得混合物。
②溶解：在不断搅拌下向混合物中加入107L纯化水，待固体完全溶解后，置3℃冷库冷藏至混合溶液温度为6℃，得溶解液。
③澄清：保持溶解液温度为6℃，环境温度8℃操作，将溶解液通过孔径为200nm的陶瓷膜成套设备澄清，进完料以后，加25L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得147kg陶瓷膜清液。
④结晶：将147kg陶瓷膜清液真空减压浓缩至36.5％固形物含量，得32.8kg浓缩液。然后冷却至室温，静置6h，析出大量白色结晶；再将结晶体系整体置1℃继续析晶，静置5h，至结晶析出完全。抽滤，分别收集结晶和母液。
⑤沸腾制粒：①将结晶干燥至含水量8％，得9.1kg，投入流化床，保持沸腾状态和中高风速，温度78℃；②将母液按每小时29kg匀速喷入；③混合均匀，得结晶颗粒。
⑥干燥：控制温度62℃，将结晶颗粒鼓风干燥，得到11.7kg罗汉果复配甜味剂。
实施例3
(1)制备秋葵幼果粘液：
①提取：取100kg秋葵幼果，用切药机破碎成宽度约4mm的长条形细块，投入1m 3搅拌罐中，以水为溶媒，在室温8℃搅拌提取。提取2次，第1次加水600L，提取2.0h；第2次加水500L，提取1.5h。每次提取完过滤，第1次提取渣再进行第2次提取。合并第1次和第2次提取液，得1100L水提取液；第2次提取后的提取渣另器收集。
②澄清：先将水提取液过碟式离心机，再过孔径为500nm的陶瓷膜成套设备澄清。进完料液后，加300L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得1300L陶瓷膜清液。
③浓缩：将陶瓷膜清液通过反渗透膜成套设备浓缩至2.3％固形物含量，得106.5kg乳白色的秋葵幼果粘液。
(2)制备秋葵浓缩汁：
①增香：将制备秋葵幼果粘液所得提取渣按以下方法烘烤，先在温度70℃烘烤至含水量45％，再在温度106℃烘烤至含水量26％，最后在温度135℃烘烤至散发出浓郁的焦香味，得8.0kg风味渣。
②提取：将8.0kg风味渣投入100L夹套搅拌罐中，以73％乙醇为溶媒，加热至61℃保温搅拌提取。提取2次，第1次加溶媒50L，提取2.0h；第2次加溶媒40L，提取1.5h。每次提取完过滤，第1次提取渣再进行第2次提取，第2次提取渣经回收乙醇后弃去。合并第1次和第2次提取液，得73L乙醇提取液。
③澄清：将提取液通过孔径为500nm的陶瓷膜成套设备澄清。进完料液后，加25L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得85L陶瓷膜清液。
④脱色：将陶瓷膜清液通过截留分子量为10KD的超滤膜成套设备脱色。进完料以后，加25L纯化水洗膜，并将上游液浓缩至7％固形物含量，得29L膜脱色液；
⑤回收乙醇：将膜脱色液通过短时真空浓缩完全回收乙醇，并浓缩至26％固形物含量，得7.8kg脱色的秋葵浓缩汁。
(3)混合、溶解、澄清：
①混合：取步骤(1)所得秋葵粘液50份、步骤(2)所得秋葵浓缩汁25份、V50罗汉果甜苷(罗汉果苷V含量52.5％)1份、赤藓糖醇200份，混合，得混合物。
②溶解：在不断搅拌下向混合物中加入211L纯化水，待固体完全溶解后，置5℃冷库冷藏至混合溶液温度为9℃，得溶解液。
③澄清：保持溶解液温度为9℃，环境温度8℃操作，将溶解液通过孔径为200nm的陶瓷膜成套设备澄清，进完料以后，加25L纯化水洗陶瓷膜上游液，合并流出液和水洗液，得253kg陶瓷膜清液。
④结晶：将253kg陶瓷膜清液真空减压浓缩至37.6％固形物含量，得52.9kg浓缩液。然后冷却至室温，静置5h，析出大量白色结晶；再将结晶体系整体置2℃继续析晶，静置6h，至结晶析出完全。抽滤，分别收集结晶和母液。
⑤沸腾制粒：①将结晶干燥至含水量11％，得16.1kg，投入流化床，保持沸腾状态和中高风速，温度76℃；②将母液按每小时21kg匀速喷入；③混合均匀，得结晶颗粒。
⑥干燥：控制温度63℃，真空度-0.09MPa，将结晶颗粒真空干燥，得到19.5kg罗汉果复配甜味剂。
实施例4
其他与实施例3相同，区别在于V50罗汉果甜苷的的用量为0.6份。
实施例5
其他与实施例3相同，区别在于V50罗汉果甜苷的的用量为2份。
实施例6
其他与实施例3相同，区别在于秋葵幼果粘液的用量为25份、秋葵浓缩汁的用量为50份。
实施例7
其他与实施例3相同，区别在于步骤(2)制备秋葵浓缩汁中，直接将提取渣在温度135℃烘烤至散发出焦香味，即没有进行温度67℃和温度106℃的烘烤。
实施例8
其他与实施例3相同，区别在于步骤(2)制备秋葵浓缩汁中，①增香：将制备秋葵幼果粘液所得提取渣按以下方法烘烤，先在温度70℃烘烤至含水量45％，再在温度106℃烘烤至含水量26％，最后在温度120℃烘烤。
实施例9
其他与实施例3相同，区别在于步骤(2)制备秋葵浓缩汁中，①增香：将制备秋葵幼果粘液所得提取渣按以下方法烘烤，先在温度70℃烘烤至含水量45％，再在温度106℃烘烤至含水量26％，最后在温度150℃烘烤，所得风味渣有一点烧糊的味道。
实施例10
其他与实施例3相同，区别在于步骤(3)混合、溶解、澄清：⑤沸腾制粒：①将结晶干燥至含水量17％。最终制备得到的产品在空气中放置一段时间，存在部分板结问题。
对比例1
其他与实施例3相同，区别在于步骤(3)中①混合中，没有加入秋葵幼果粘液，同时秋葵浓缩汁的用量为75份。
对比例2
其他与实施例3相同，区别在于步骤(3)中①混合中，没有加入秋葵浓缩汁，同时秋葵幼果粘液的用量为75份。
应用例
将上述实施例和对比例所得的复配甜味剂用矿泉水调配成水溶液，稀释的倍数是使稀释后的水溶液甜度和5％蔗糖水溶液接近，即甜度接近1。之后进行如下测试，结果列于表1：
1.感官分析人员的筛选与培训
根据GB/T 16291.2-2010的规定来筛选感官评定人员，经过口味敏感性培训后，最终筛选20名(男女各半)的感官评价人员，组成感官评定小组。
2.甜味持续时间：请受试人员品尝稀释至甜度接近5wt％蔗糖溶液的复配甜味剂水溶液，并以5wt％蔗糖溶液为对照组，从评定人员喝下开始计时，记录受试者感觉甜味消失的时间，排除那些品尝5wt％蔗糖溶液的甜味持续时间偏离5秒超过1秒的受试者的数据，即排除那些品尝5wt％蔗糖溶液的甜味持续时间小于4秒和大于6秒的受试者的数据。最终所得平均值为本发明复配甜味剂的甜味持续时间。
3.口感主观评价：
感官分析人员在评定实验开始前1h内限制饮食，尤其是能严重影响味觉的食物。针对不同味感实验从20名中选取12名最合适的感官分析人员进行的复配甜味剂溶液的感官评定。针对甜味剂的溶液的气味和口感进行综合打分评价，分值为1分至10分，以5wt％蔗糖溶液作为参照，5％蔗糖溶液满意度最高为10分，最低为1分，每次调查问卷测试人员为12人，去掉一最高分值，去掉一最低分值，最后求其整体的平均值。
将测试样品分为复配组和对照组，复配组为实施例中按照配方得到的复配组合物产品，对照组为5wt％蔗糖溶液，取10mL待评定溶液于一次性纸杯中，由感官评定人员含于口中，停留数秒吐出，评定时间间隔为20min，评定结果取10名评定人员打分的平均值。对照组的感官评定标准为10分满分。
此外还对复配的甜味剂的板结情况进行测试：将实施例和对比例所得的复配甜味剂在25℃，65RH％条件下存放24h，测试吸潮率和是否出现板结情况。对照组是以市购蔗糖作为试验物质。
表1
Figure PCTCN2021072429-appb-000001
Figure PCTCN2021072429-appb-000002
Figure PCTCN2021072429-appb-000003
通过表1数据可知，本发明利用来自秋葵的两种原料，即秋葵粘液和秋葵幼果粘液提取渣烘焙后提取得到秋葵浓缩汁，和罗汉果提取物，赤藓糖醇复配后得到的复配甜味剂，能够有效缩短罗汉果提取物的甜味持续时间，也即，改善了基于罗汉果的甜味剂的后甜味问题，从而扩宽了罗汉果提取物作为甜味复配剂中的用途，提高了罗汉果的经济价值。而且，本发明得到的复配甜味剂不仅解决了罗汉果提取物的后甜味问题，通过特定的烘焙工艺，还使复配甜味剂带有特殊的果香味，改善了甜味剂的口感。

Claims (10)

  1. 一种改善罗汉果提取物持久甜味和甜度倍数的复配甜味剂，其制备方法中采用的原料包括：秋葵幼果粘液，秋葵浓缩汁，罗汉果提取物、赤藓糖醇，条件是罗汉果提取物中罗汉果甜苷V的质量为秋葵幼果粘液和秋葵浓缩汁总质量的0.3-1％。
  2. 根据权利要求1所述的复配甜味剂，其特征在于，所述复配甜味剂把包括以下质量份的原料：30-50份秋葵幼果粘液，15-25份秋葵浓缩汁，1-30份罗汉果提取物、100-500份赤藓糖醇。
  3. 根据权利要求1或2所述的复配甜味剂，其特征在于，罗汉果提取物中罗汉果甜苷V的质量为秋葵幼果粘液和秋葵浓缩汁总质量的0.5-0.8％。
  4. 根据权利要求1或2所述的复配甜味剂，其特征在于，秋葵幼果粘液中固形物的含量为2-10％，优选4-7％；秋葵浓缩汁中固形物的含量为20-30％。
  5. 根据权利要求1或2所述的复配甜味剂，其特征在于，所述秋葵幼果粘液是通过包括以下步骤的制备方法得到：秋葵幼果用水提取，收集提取渣和提取液，提取液过滤后浓缩得到秋葵幼果粘液。
  6. 根据权利要求5所述的复配甜味剂，其特征在于，所述秋葵幼果为花谢后4～7天即应采收；提取的温度是8-30℃，优选8-15℃。
  7. 根据权利要求1或2所述的复配甜味剂，其特征在于，所述秋葵浓缩液是通过包括以下步骤的制备方法得到：取秋葵幼果粘液制备过程中的提取渣，进行烘焙后得到风味渣，风味渣用醇水溶液提取，经过过滤，脱色，浓缩得到秋葵浓缩液。
  8. 根据权利要求7所述的复配甜味剂，其特征在于，所述烘焙是在130-140℃下进行，烘焙时间为0.5-1.5h；
    优选地，在进行烘焙前，先进行60-100℃的脱水处理；
    更优选地，所述脱水处理，是提取渣先在60-75℃下烘烤0.5-1h，使含水量在50％以下，再在90-110℃下烘烤0.5-1h，使含水量在30％以下。
  9. 根据权利要求1或2所述的复配甜味剂，其特征在于，所述过滤是通过陶瓷膜得澄清液；所述脱色是通过超滤膜，截留分子量为8KD～30KD，所述浓缩是反渗透浓缩或真空浓缩。
  10. 权利要求1-9任一项所述复配甜味剂的制备方法，包括以下步骤：将秋葵粘液、秋葵脱色风味浓缩汁、罗汉果提取物、赤藓糖醇按一定比例混合，溶解，过滤，结晶， 沸腾制粒，干燥即得；优选地，在沸腾制粒前，对结晶所得晶体进行干燥至含水量＜15％。
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