阅读说明：本技术 一种破壁提取山姜素的制备方法 (Preparation method for extracting alpinetin by breaking cell walls ) 是由 杨成东 于 2018-05-30 设计创作，主要内容包括：本发明涉及一种破壁提取山姜素的制备方法,其步骤如下：取山姜根状茎洗净、干燥、粉碎,过40目筛,粉末浸泡于乙醇中,浸泡好的材料加入到超高压提取器中,利用超高压和撞击流技术提取山姜中的山姜素；经提取后的山姜素上大孔吸附树脂,采用体积比为20:1的氯仿-甲醇溶液洗脱,收集洗脱液,减压浓缩,得浓缩物；将浓缩物采用高速逆流色谱法分离纯化,以氯仿-甲醇-水为两相溶剂系统,取上相做固定相、下相为流动相,主机转速800-1000rpm,流速为2-3mL/min,收集目标流分,回收试剂,干燥即可得到产品。本发明方法样品损耗少,分离效果好,成本低廉,能得到含量高、品质好的山姜素。(The invention relates to a preparation method for extracting alpinetin by breaking walls, which comprises the following steps: cleaning rhizome of Alpinia japonica, drying, pulverizing, sieving with 40 mesh sieve, soaking the powder in ethanol, adding the soaked material into an ultrahigh pressure extractor, and extracting alpinetin from Alpinia japonica by ultrahigh pressure and impinging stream technology; loading the extracted alpinetin on macroporous adsorbent resin, eluting with chloroform-methanol solution at volume ratio of 20:1, collecting eluate, and concentrating under reduced pressure to obtain concentrate; separating and purifying the concentrate by adopting a high-speed counter-current chromatography, taking chloroform-methanol-water as a two-phase solvent system, taking an upper phase as a stationary phase and a lower phase as a mobile phase, collecting target fractions, recovering a reagent, and drying to obtain the product, wherein the rotation speed of a host is 800-1000rpm, and the flow speed is 2-3 mL/min. The method has the advantages of less sample loss, good separation effect, low cost and capability of obtaining the alpinetin with high content and good quality.)

1. A preparation method for extracting alpinetin by breaking walls is characterized by comprising the following steps:

a. Cleaning rhizoma Alpiniae Officinarum rhizome, drying, pulverizing, sieving with 40 mesh sieve, soaking the powder in ethanol, adding the soaked material into an ultrahigh pressure extractor, and extracting alpinetin from rhizoma Alpiniae Officinarum by ultrahigh pressure and impinging stream technology.

b. loading the extracted alpinetin on macroporous adsorbent resin, eluting with chloroform-methanol solution at volume ratio of 20:1, collecting eluate, and concentrating under reduced pressure to obtain concentrate;

c. separating and purifying the concentrate by adopting a high-speed counter-current chromatography, taking chloroform-methanol-water as a two-phase solvent system, taking an upper phase as a stationary phase and a lower phase as a mobile phase, collecting target fractions, recovering a reagent, and drying to obtain the product, wherein the rotation speed of a host is 800-1000rpm, and the flow speed is 2-3 mL/min.

2. The method as claimed in claim 1, wherein the pressure in step a is 200-300MPa and the temperature is normal temperature.

3. The method for preparing wall-broken alpinetin according to claim 1, wherein the macroporous adsorbent resin in step b is any one of AB-8, D-101, and DA-201.

4. The method for preparing wall-broken alpinetin according to claim 1, wherein the mass ratio of the resin amount to the raw materials in step b is 1: 2.

5. The method for preparing wall-broken alpinetin according to claim 1, wherein the chloroform-methanol-water volume ratio in step c is 10:5: 6.

Technical Field

The invention relates to a preparation method for extracting alpinetin by breaking walls, belonging to the field of extraction of effective components of traditional Chinese medicines.

background

The rhizoma Alpiniae Officinarum is prepared from rhizome of Alpinia of Zingiberaceae by collecting, cleaning, and sun drying in 3-4 months. Dispel wind, dredge collaterals, regulate qi and alleviate pain. The alpinetin extracted from rhizoma Alpiniae Officinarum has antibacterial, antioxidant, anticancer, antithrombotic, blood pressure lowering, blood lipid reducing, blood glucose reducing, antiemetic, and analgesic effects. Can be used for treating rheumatic arthritis, traumatic injury, toothache, and gastralgia.

At present, water decoction method, percolation method and the like are mostly adopted for extracting the alpinetin, the traditional extraction method consumes time and has low extraction rate, the ultrahigh pressure impinging stream technology is adopted and the macroporous resin adsorption and purification technology is combined, so that the extraction rate of the alpinetin can be effectively improved, the loss of effective components is reduced, and the content of pesticide residues in medicinal materials is reduced.

Disclosure of Invention

aiming at the defects of the prior art, the invention aims to provide a method for preparing the alpinetin, which has high efficiency and selectivity, is simple and convenient to operate, has high yield and few byproducts and can be industrially realized.

The technical scheme of the invention is carried out according to the following steps:

a. Drying and crushing the alpinia japonica medicinal material, sieving the crushed alpinia japonica medicinal material by a 40-mesh sieve, soaking the powder in ethanol, adding the soaked material into an ultrahigh pressure extractor, and extracting the alpinia japonica extract in the alpinia japonica by utilizing ultrahigh pressure and impinging stream technology;

b. Loading the extracted alpinetin on macroporous adsorbent resin, eluting with chloroform-methanol solution at volume ratio of 20:1, collecting eluate, and concentrating under reduced pressure to obtain concentrate;

c. Separating and purifying the concentrate by adopting a high-speed counter-current chromatography, taking chloroform-methanol-water as a two-phase solvent system, taking an upper phase as a stationary phase and a lower phase as a mobile phase, collecting target fractions, recovering a reagent, and drying to obtain the product, wherein the rotation speed of a host is 800-1000rpm, and the flow speed is 2-3 mL/min.

The pressure in the step a is 200-300MPa, and the temperature is normal temperature.

The type of the macroporous absorption resin in the step b is any one of AB-8, D-101 and DA-201.

The mass ratio of the resin dosage to the raw materials in the step b is 1: 2.

And c, the volume ratio of chloroform-methanol-water in the step c is 10:5: 6.

The present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.

The specific implementation mode is as follows: