阅读说明：本技术 一种用大孔吸附树脂纯化罗汉果甜苷v的方法 (Method for purifying mogroside V by using macroporous adsorption resin ) 是由 张泽生 刘暄 于 2019-09-27 设计创作，主要内容包括：本发明涉及一种大孔吸附树脂纯化罗汉果甜苷V的方法,利用大孔吸附树脂对市售含40％罗汉果甜苷V的罗汉果甜苷混合物进行吸附,再对其进行后处理得到纯化的罗汉果甜苷V。本发明的纯化方法得到的罗汉果甜苷V提取物得率为70％～80％,有效成分含量高、杂质少,纯度在70％以上。该方法安全稳定且成本低廉,可重复利用。因此,适合于工厂大规模生产实践,便于实际生产。(The invention relates to a method for purifying mogroside V by using macroporous adsorption resin, which is characterized in that the macroporous adsorption resin is used for adsorbing a mogroside mixture containing 40% of mogroside V sold in the market, and the purified mogroside V is obtained by post-treating the mixture. The mogroside V extract obtained by the purification method has the yield of 70-80 percent, high content of effective components, less impurities and purity of more than 70 percent. The method is safe, stable, low in cost and reusable. Therefore, the method is suitable for large-scale production practice in factories and is convenient for actual production.)

1. A method for purifying mogroside V by using macroporous adsorption resin comprises the following steps:

s1, macroporous adsorption resin pretreatment: soaking macroporous adsorption resin in ethanol for 24h → washing with ethanol until the effluent liquid is not turbid → washing with water until no alcohol smell exists → soaking with 5% HCL for 2-4 h → washing with water until the effluent liquid is neutral → soaking with 2% NaOH for 2-4 h → washing with water until the effluent liquid is neutral, and loading the macroporous adsorption resin into an adsorption column for later use;

s2, dissolving mogroside in purified water to obtain a mogroside mixed solution, and loading the mogroside mixed solution through an adsorption column;

s3, after sample loading, washing with water with 2 times of column volume to remove non-adsorbates;

s4, performing primary elution by adopting 20% ethanol with 5 times of column volume to remove part of high molecular weight mogrosides;

s5, performing secondary elution by adopting ethanol with concentration of 40% and 10 times of column volume;

s6, collecting the eluent obtained in the step S5, concentrating and drying to obtain a product containing mogroside V with the purity of 70%;

s6, performing three-time elution by adopting 60% ethanol with 5 times of column volume so as to recycle the macroporous resin;

s7, the yield of the mogroside V extract obtained by the purification method is 70-80%, and the mogroside V extract has high content of effective components and few impurities.

2. The method of purifying mogroside V by using macroporous adsorbent resin as claimed in claim 1, wherein the macroporous adsorbent resin in step S1 is HZ-806.

3. The method for purifying mogroside V by using macroporous adsorbent resin as claimed in claim 1, wherein the mogroside in step S2 is commercially available mogroside V containing 40%.

4. The method for purifying mogroside V by using macroporous adsorbent resin as claimed in claim 1, wherein the sample loading amount in step S2 is 10g/100g wet weight packing, and the sample loading flow rate is 1.5 BV/h.

5. The method for purifying mogroside V by using macroporous adsorbent resin as claimed in claim 1, wherein the flow rate of water in step S3 is 1 BV/h.

6. The method for purifying mogroside V by using macroporous adsorbent resin as claimed in claim 1, wherein the flow rate of the eluent in steps S4, S5 and S7 is 1 BV/h.

7. The method of purifying mogroside V using macroporous adsorbent resin as claimed in claim 1, wherein:

(1) the macroporous adsorption resin adopted in the method is HZ-806, which is mostly applied to natural product extraction and has the advantages of safety, stability, low cost, reusability and the like;

(2) the purification process of the mogroside V is simple and convenient to operate and high in efficiency, the yield can reach 70% -80%, and the purity of the mogroside V is over 70%;

(3) the method is suitable for large-scale production practice in factories and is convenient for actual production.

Technical Field

The invention relates to a method for purifying mogroside V by macroporous adsorption resin, in particular to a process method suitable for purifying mogroside V in actual production in a factory.

Background

Mogroside is composed of a group of triterpene aglycone connected with 2-6 glycosyl glycoside, also called mogroside and mogroside, is a non-sugar substance with strong sweet taste, and has the characteristics of low heat, light color, strong water solubility and stability and the like. Mainly comprises a plurality of triterpenoid components such as mogroside III, IV, V and the like, wherein the mogroside V is a sweetener which has pure sweet taste and does not influence the blood sugar content of normal people and is safe. In recent years, the effect of mogroside V on treating and preventing diabetes and complications thereof is widely concerned by various national scholars, and the mogroside V is found to delay the absorption of carbohydrates, reduce postprandial blood sugar, promote insulin secretion and have the effect of preventing and treating the diabetes complications.

Most of products for producing mogroside are mixtures of mogroside, and the relative content of mogroside V is not high, so the invention relates to a method for purifying mogroside V by adopting macroporous adsorption resin, which is suitable for actual production in factories, so as to develop products with high content of mogroside V.

Disclosure of Invention

The method for purifying mogroside V by using macroporous adsorption resin takes macroporous adsorption resin as an adsorbent, adsorbs a commercial mogroside mixture containing 40% of mogroside V, and then carries out post-treatment on the mixture to obtain the purified mogroside V. The invention aims to provide a process method suitable for actually producing mogroside V in a factory, so as to improve the purity of the mogroside V in large-scale production, and the process is simple, convenient and feasible and has low cost.

In order to achieve the purpose, the invention adopts the technical scheme that:

s1, the macroporous adsorption resin is HZ-806 macroporous adsorption resin. The resin is milky white or light blue opaque spherical particles, the water content is 68-78%, the wet density (20 ℃) is 1.02-1.12 g/mL, the wet apparent density is 0.70-0.80 g/mL, and the particle size range is 0.315-1.25 mm. The HZ-806 macroporous adsorbent resin is a macroporous medium-polarity adsorbent, and is suitable for extraction and purification of natural products, extraction of Chinese herbal medicines, extraction of antibiotics and the like by means of Van der Waals force. Has the advantages of good mechanical strength, simple and convenient operation, regeneration and repeated use, and the like.

Pretreating macroporous adsorption resin HZ-806: soaking the macroporous adsorption resin in absolute ethyl alcohol for 24h → washing with absolute ethyl alcohol until the effluent liquid and water are in a ratio of 1: 5 and are not turbid → washing with water until no alcoholic smell exists → soaking with 5% HCL for 2-4 h → washing with water until the macroporous adsorption resin is neutral → soaking with 2% NaOH for 2-4 h → washing with water until the macroporous adsorption resin is neutral for later use;

s2, loading the pretreated macroporous adsorption resin HZ-806 in the S1 into an adsorption column, dissolving commercially available mogroside V containing 40% of mogroside V in purified water to obtain a mogroside mixed solution, and loading at the flow rate of 1.5BV/h, wherein the loading amount is 10g/100g of wet weight filler;

s3, after sample loading, washing the macroporous adsorption resin packed column with 2 times of column water at the flow rate of 1BV/h to remove impurities;

s4, after water washing, eluting the macroporous adsorption resin packed column, and performing primary elution by adopting 20% ethanol with 5 times of column volume at the flow rate of 1BV/h to remove part of high molecular weight mogrosides;

s5, performing secondary elution by adopting 10 times of column volume of 40% ethanol at the flow rate of 1BV/h, collecting eluent, concentrating and drying the eluent to obtain a product containing the mogroside V with the purity of more than 70%.

S6, performing three times of elution by using 60% ethanol with 5 times of column volume at the flow rate of 1BV/h, and thoroughly cleaning the macroporous adsorption resin so as to recycle the macroporous adsorption resin at a later stage;

s7, the mogroside V extract obtained by the purification method has the yield of 70-80%, high content of effective components, less impurities and purity of more than 70%, and is suitable for purifying the mogroside V in actual production of factories.

Compared with the prior art, the invention has the advantages that:

(1) the macroporous adsorption resin adopted in the method is HZ-806, which is mostly applied to natural product extraction and has the advantages of safety, stability, low cost, reusability and the like;

(2) the purification process of the mogroside V is simple and convenient to operate and high in efficiency, the yield can reach 70% -80%, and the purity of the mogroside V is over 70%;

(3) the method is suitable for large-scale production practice in factories and is convenient for actual production.

Detailed Description

The present invention will be described in further detail with reference to examples.

The raw materials are all commercial products.

Example 1:

a method for purifying mogroside V by using macroporous adsorption resin comprises the following steps:

(1) loading 90g of pretreated HZ-806 macroporous adsorption resin into an adsorption column;

(2) accurately weighing 9g of a commercially available mogroside mixture containing 40% mogroside V, pouring the mixture into a container, adding 180mL of purified water, and stirring until the mixture is clear to obtain a sample solution;

(3) loading the mogroside aqueous solution containing 40% of mogroside V through an adsorption column at the flow rate of 1.5 BV/h;

(4) passing 2 times of column volume of purified water through the adsorption column at a flow rate of 1BV/h to remove non-adsorbates;

(5) passing 20% ethanol of 5 times column volume through adsorption column at flow rate of 1BV/h for one time to remove high molecular weight mogrosides;

(6) carrying out secondary elution on 40 percent ethanol with 10 times of column volume by passing through an adsorption column at the flow rate of 1 BV/h;

(7) and (4) carrying out rotary evaporation on the organic solution adsorbed in the step (6) at 40 ℃ and 0.7Mpa, and drying in a 60 ℃ forced air drying oven for 5 hours after rotary drying. The yield of the obtained product is 77.63%, and the purity of the mogroside V is 70.28%.

(8) Three elutions were carried out with 5 column volumes of 60% strength ethanol at a flow rate of 1BV/h through the adsorption column for later reuse of the macroporous adsorbent resin.

While the invention has been described in connection with a preferred embodiment, it is not intended to limit the invention, and it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention.