CN102058626A

CN102058626A - Method for extracting effective components from hippochaete ramosissimum

Info

Publication number: CN102058626A
Application number: CN201010579985XA
Authority: CN
Inventors: 李锦宇; 陈莉华; 张俊生
Original assignee: Individual
Current assignee: Individual
Priority date: 2010-12-09
Filing date: 2010-12-09
Publication date: 2011-05-18

Abstract

The invention relates to a method for extracting general flavones, total alkaloids, organosilicate, polishing agent and other effective components from hippochaete ramosissimum. The method comprises the following steps of: drying overground parts of hippochaete ramosissimum plants in the shade and preparing into medicinal material coarse powder with a plant pulverizer; adding 70-80% alcohol used as a solvent in a certain proportion, processing with ultrasound, dipping and then carrying out reduced-pressure concentrating on filtrate, recycling the alcohol, and extracting organosilicate from filter residues; absorbing and eluting the filtrate to obtain general flavones; neutralizing water eluent with alkali and reextracting with sulfuric acid to prepare nicotine; carrying out microwave assistance, strong acid hydrolysis and organic regent extraction on filter residues obtained in a material pretreatment stage to prepare organosilicate; cleaning, filtering and drying filter residue scraps, spreading super glue on the filter residue scraps evenly for fixing and forming to obtain a natural environment-friendly wood ware and metal polishing agent. The method can be used for extracting general flavones, total alkaloids, organosilicate and polishing agent from hippochaete ramosissimum with simple process, low cost and high yield.

Description

A kind of method of from Herba Clinopodii Polycephali, extracting active ingredient

Technical field

The present invention relates to a kind of method of from Herba Clinopodii Polycephali, extracting active ingredient.

Background technology

" Chinese pharmacopoeia record, the Herba Equiseti Hiemalis claims file grass, nib grass, Herba equiseti ramosissimi, Herba Clinopodii Polycephali again, is the dry aerial parts of Equisetaceae plant Herba Equiseti Hiemalis Equisetum hiemale L., is born in the dark and damp place of hillside sylvan life, riparian wetland, small stream limit, like dark and damp environment, also be born in weeds ground sometimes.Nature and flavor are sweet, bitter, and are flat.Belong to lung, Liver Channel.Diffusing wind heat is arranged, move back the effect of corneal nebula, be used for the wind heat conjunctival congestion, epiphora induced by wind, order is given birth to nebula.Aerial parts contains four big constituents: a class is organic acid such as succinic acid, Fumaric acid, P-hydroxybenzoic acid, m-hydroxybenzoic acid, ferulic acid etc.; Second largest class is to contain flavonoid glycosides material such as kaempferol, Quercetin, luteolin and their glycoside etc.; The third-largest class is for containing alkaloid such as equisetine, nicotine etc.; The fourth-largest class is silicon dioxide, organosilicate of phosphate, volume etc.

Flavone compound has multiple biological activity, can blood pressure lowering, analgesia, antibiotic, heat-clearing and toxic substances removing, inhibition lipoxidase, anticancer etc., to treatment coronary heart disease, delay atherosclerosis and eliminate aspects such as free radical that remarkable result is arranged; Alkaloid has antibacterial and anti-inflammation functions; Organosilicate helps to repair fracture and forms this class of collagen and is present in key protein in connective tissue, skin, skeleton, cartilage and the ligament.

The relevant report that Flavonoid substances extracts in the domestic existing Herba Clinopodii Polycephali, but seldom with the whole researchs that utilize of the effective ingredient in the Herba Clinopodii Polycephali, because the advantage of Wuling mountain area weather conditions, Herba Clinopodii Polycephali at the dark and damp place of hillside sylvan life, riparian wetland, small stream limit, dark and damp environment even weeds ground all can grow, even have influence on the normal Nutrient Absorption of field-crop, if can be with it comprehensive utilization, not only solve the influence of farmland weed to crops, and make it to turn waste into wealth, for poor areas of the western region peasant opens up new road of getting wealth.

Summary of the invention

The present invention aims to provide a kind of method of extracting active ingredients such as total flavones, total alkaloids, organosilicate and buffing compound from Herba Clinopodii Polycephali continuously.

Method of the present invention may further comprise the steps:

Pretreatment of raw material: selection is grown fine, the Herba Clinopodii Polycephali above-ground plant parts of healthy no disease and pest, and the back of drying in the shade is made medicinal material coarse powder and put into former pocket standby with the plant pulverizer.

Above-mentioned medicinal material coarse powder 70-80% ethanol adds solvent by 1: 10 solid-liquid ratio, and ultrasonic 2 hours, in 60 ℃ of dippings after 16-24 hour, isolated by filtration liquid and solid, filtrate decompression concentrates and reclaims ethanol, and filtering residue is used to extract organosilicate.

1) ultrasound wave is assisted-ethanol extraction-macroporous adsorbent resin separation preparation total flavones:

Above-mentioned filtrate is removed various plant pigment with petroleum ether extraction, by AB-8 type macroporous adsorbent resin, water, 95% ethanol elution successively, water elution liquid gives over to extract total alkaloids usefulness, and ethanol elution reclaims ethanol to doing, and obtains total flavones.Yield is 1.16%.

Detection method: with according to state-promulgated pharmacopoeia, be the check and inspection flavones content with the kaempferide, purity is 90-95%.

2) alkali neutralization-sulphuric acid is stripped and is prepared nicotine

Above-mentioned water elution liquid is concentrated, add a certain amount of 0.5%NaOH solution by 1: 20 solid-liquid ratio, place 65 ℃ of ultrasonic water bath to react 3h, filter the back and regulate gained filtrate pH to 12, extract 3 time at 1: 2 according to volume ratio with normal hexane, organic facies is with 20% sulfuric acid solution back extraction, after regulating pH to 12, use the normal hexane reextraction, obtain total alkaloids after the distilling under reduced pressure, yield 3%, wherein nicotine content is 45%.The normal hexane recycle and reuse.

Detection method 1: press ISO 13276-1997 national standard, measure the purity of nicotine with the tungstosilicic acid gravimetry.

Detection method 2: the nicotine neutral sulfate. in the ultraviolet spectrophotometry analytic product of adopting international standards to recommend or the content of natural nicotine, according to being that the nicotine aqueous solution exists characteristic absorption peak at the 259nm place, measure 236nm, 259nm, the absorbance D at 282nm 3 places ₂₃₆, D ₂₅₉, D ₂₈₂, calculate the purity of natural nicotine by following formula:

Nicotine content %=1.059 * F * [D ₂₅₉-1/2 (D ₂₃₆+ D ₂₈₂)] * V * 100/34.3 * nicotine gross mass

3) microwave-assisted-strong acid hydrolysis-organic solvent extracting prepares organosilicate

The filtering residue that the pretreatment of raw material stage is obtained was with clear water rinsing 1-2 time, and eluent is used to reclaim ethanol, and the filtering residue after the cleaning adds a certain amount of 72% H by 1: 10 solid-liquid ratio ₂SO ₄, heating 10-15min makes the mixed liquor hydrolysis, isolated by filtration liquid and solid, filtering residue are used for step preparation buffing compound down, and filtrate concentrates, obtain organosilicate after adding moisture dioxane extrct delignification by 1: 2 solid-liquid ratio, yield about 13%, purity are siliceous more than 7%.

Detect: measure silicone content with gravimetric method and the coupling of silicon molybdenum blue colorimetry.

4) make buffing compound:

Filtering residue chip in the last step is cleaned filter do, drying is evenly elaborated it on 600# or 1000# body paper deadlocked fixed-typely with strong adhesive, obtain woodenware, the medal polish agent of natural environmental-protective.

Detect: the sand paper by corresponding specification detects.

Extract total flavones, total alkaloids, organosilicate and buffing compound continuously with method of the present invention from Herba Clinopodii Polycephali, technology is simple, and cost is low, the yield height.

Specific embodiments

With the Herba Clinopodii Polycephali above-ground plant parts, the back of drying in the shade is made medicinal material coarse powder and puts into former pocket standby with the plant pulverizer.

Get above-mentioned medicinal material coarse powder 10kg and add 80% ethanol 100kg by 1: 10 solid-liquid ratio, ultrasonic 2 hours, 60 ℃ flooded after 16 hours, isolated by filtration liquid and solid, and filtrate being used to prepares total flavones and total alkaloids, and filtering residue is used to extract organosilicate.

1) ultrasound wave is assisted-ethanol extraction-macroporous adsorbent resin separation preparation total flavones

Above-mentioned filtrate (alcohol extract) is conveyed in the oil water separator, add petroleum ether in 1: 2 ratio and remove pigment, separate biphase, organic facies reclaim under reduced pressure ether utilizes again, the solution pressure-raising of water is transported to AB-8 type macroporous adsorbent resin detached dowel from gravity tank in gravity tank, make alcohol extract cross post, cross liquid behind the post and cross post once more effective ingredient is fully adsorbed, the water eluting also is positioned in the water elution liquid storage tank; Ethanol elution macroporous adsorbent resin detached dowel with 95% obtains ethanol elution and is stored in the alcohol eluen storage tank, and this liquid is delivered to vacuum concentration pan, decompression recycling ethanol concentrates near doing, and obtains the total flavones powder, carry out finished product packing after the cold drying, obtain total flavones in the Herba Clinopodii Polycephali.According to state-promulgated pharmacopoeia, be that the qualified back of check and inspection flavones content packing is dispatched from the factory with the kaempferide.

2) alkali neutralization-sulphuric acid is stripped and is prepared nicotine

Above-mentioned water elution liquid is concentrated, add a certain amount of 0.5%NaOH solution by 1: 20 solid-liquid ratio, after placing 65 ℃ of ultrasonic water bath reaction 3h, be concentrated into 1/3 of original volume at vacuum concentration pan, regulate pH to 12 with NaOH, divide 2 times and add normal hexane, the volume of adding is 2 times of total concentrated solution volume, merge n-hexane extract twice, divide 2 times and add H ₂SO ₄Strip, the volume of adding is 2 times of n-hexane extract volume, merges 2 times H ₂5O ₄Water volume after the reextraction, the normal hexane reclaim under reduced pressure of organic facies is utilized again, and water places vacuum concentration pan to concentrate, and obtains total alkaloids, is that standard substance detect and dispatch from the factory after qualified with nicotine.

The filtering residue that the pretreatment of raw material stage is obtained was with clear water rinsing 1-2 time, and eluent is used to reclaim ethanol, and the filtering residue after the cleaning adds a certain amount of 72% H by 1: 10 solid-liquid ratio ₂SO ₄Heating 10-15min, make the mixed liquor hydrolysis, isolated by filtration liquid and solid, filtering residue is used for step preparation buffing compound down, and filtrate concentrates, and adds moisture dioxane extrct delignification by 1: 2 solid-liquid ratio, divide and add moisture dioxane extracting lignin 2 times, the cumulative volume of moisture dioxane is 2 times of strong acid hydrolyzed solution, promptly in 1: 2 ratio adding, tells water, the moisture dioxane of organic facies reclaim under reduced pressure utilizes again, merge 2 times isolating water, it is dried to place vacuum concentration pan to be concentrated into, and pulverizes evenly, obtaining organosilicate, is that standard detection is dispatched from the factory after qualified with the silicone content.

4) make polishing sand paper

Filtering residue chip in the last step is cleaned filter do, drying is evenly elaborated it on 600# or 1000# body paper deadlocked fixed-typely with strong adhesive, obtain woodenware, the medal polish sand paper of natural environmental-protective.Detect by the sand paper of corresponding specification and to dispatch from the factory after qualified.

Claims

1. method of from Herba Clinopodii Polycephali, extracting active ingredient, with the Herba Clinopodii Polycephali above-ground plant parts dry in the shade the back make medicinal material coarse powder with the plant pulverizer, use 70-80% ethanol, add solvent by 1: 10 solid-liquid ratio, ultrasonic 2 hours, in 60 ℃ the dipping 16-24 hour after, isolated by filtration liquid and solid, filtrate decompression concentrates and reclaims ethanol, and filtering residue is used to extract organosilicate; It is characterized in that:

Above-mentioned filtrate is removed various plant pigment with petroleum ether extraction, by AB-8 type macroporous adsorbent resin, water, 95% ethanol elution successively, water elution liquid gives over to extract total alkaloids and uses, ethanol elution reclaims ethanol to doing, and obtains total flavones, and yield is 1.16%;

2) 2) alkali neutralization-sulphuric acid is stripped and is prepared nicotine:

Above-mentioned water elution liquid is concentrated, add a certain amount of 0.5%NaOH solution by 1: 20 solid-liquid ratio, place 65 ℃ of ultrasonic water bath to react 3h, filter the back and regulate gained filtrate pH to 12, extract 3 time at 1: 2 according to volume ratio with normal hexane, organic facies is with 20% sulfuric acid solution back extraction, after regulating pH to 12, use the normal hexane reextraction, obtain total alkaloids after the distilling under reduced pressure, yield 3%, wherein nicotine content is 45%;

3) microwave-assisted-strong acid hydrolysis-organic solvent extracting prepares organosilicate:

The filtering residue that the pretreatment of raw material stage is obtained was with clear water rinsing 1-2 time, and eluent is used to reclaim ethanol, and the filtering residue after the cleaning adds a certain amount of 72% H by 1: 10 solid-liquid ratio ₂SO ₄, heating 10-15min makes the mixed liquor hydrolysis, isolated by filtration liquid and solid, and filtrate concentrates, and obtains organosilicate after adding moisture dioxane extrct delignification by 1: 2 solid-liquid ratio, and yield 13%, purity are siliceous more than 7%;

4) make buffing compound:

The filtering residue chip is cleaned, filter is done, dry, with strong adhesive it is evenly elaborated on body paper deadlocked fixed-typely, obtain woodenware, the medal polish agent of natural environmental-protective.