CN101220013A - Method for extracting and separating meletin from Mesona Procumbens Hemsl - Google Patents

Abstract

The invention discloses a method for extracting quercetin from all-grass of grass jelly, which comprises the following steps: (1) getting a plurality of all-grass of grass jelly, adding 20 times of water to boil and extract, slowly adding limewater during agitation until the pH is 8 to 9, then adding 3 percent of boric acid and boiling for 20 to 30 minutes under the pH condition; (2) filtering before getting cold, repeatedly depressurizing and filtering the residue for 3 times and combining the filtrate; under the condition of 60 to 70 DEG C, adjusting combined liquid to pH value of 5 by concentrated hydrochloric acid, pumping the acid liquid after placing for 24 hours; (3) washing the precipitate to be neutral by water, drying at the temperature of 60 DEG C to derive rutin crude product, recrystallizing by boiling water, and drying in 70 to 80 DEG C to derive the rutin pure product; (4) adding 2 percent of H2SO4 to the refined rutin by a proportion of 1:80, heating with fire for 2 hours, cooling and pumping; (5) washing the residual water to be neutral, and then implementing 95 percent ethanol recrystallization and sephadex chromatography separation (SphadexLH20), using carbinol as an eluant; (6) deriving quercetin yellowish green pure product as the rutin can not be eluted. The method for extracting quercetin from all-grass of grass jelly has the advantages of simplicity, low cost and high yield, which is suitable for industrial production.

Description

A kind of from the careless herb of celestial being the method for extraction separation Quercetin

Technical field:

The invention discloses a kind of from plant Mesona the method for extraction separation Quercetin.

Background technology:

Celestial grass has another name called Herba mesonae chinensis, the Mesona chinensis Benth, and the celestial being is frozen, and firewood grass etc. are for the celestial grass of Labiatae belongs to the annual herb plant.Celestial careless herb dry sample contains 70% carbohydrate of having an appointment, and a small amount of protein, fat, pigment etc. also contain more mineral element.In the careless contained functional ingredient of celestial being, ursolic acid can reducing blood-fat, also can liver lipid lowering, and be fat-reducing liver-protecting medicine with potentiality to be exploited, or main whitening composition in the cosmetics; Quercetin have preferably eliminate the phlegm, antitussive action, and certain antiasthmatic effect arranged, bring high blood pressure down, strengthen capillary resistance in addition in addition, reduce capillary fragility, reducing blood-fat, coronary artery dilator, effects such as coronary blood flow increasing, be used for the treatment of chronic bronchitis, coronary heart disease and hyperpietic are also had the assisting therapy effect; Essence have the effect of calmness, refreshing and detoxicating Li Shui; Trace element has and suppresses that free radical forms, anti-ageing, anticancer effect; Physiological function etc. can be regulated and strengthen to VITAMIN.

Celestial grass is cold in nature, sweet, light, cool, and is medicinal extensive, and clearing heat and promoting diuresis, the effect of cool blood relieving summer-heat are arranged.Be used for acute rheumatic arthritis, heatstroke, heat poison, quench one's thirst, hypertension, nephropathy, diabetes, pain of joint muscle, wine wind, gonorrhoea etc.

Be that the series product of development of raw materials have with celestial grass at present: the careless agar of instant celestial being, celestial careless health tea, celestial careless cola beverages, instant celestial grass, celestial being's plate etc., these products mainly are to be that the celestial herb rubber of solvent extraction is the product that raw material is made with water.Because can not be water-soluble, have preferably eliminate the phlegm, antitussive action, and have the Quercetin of certain antiasthmatic effect to be present in to extract and be taken as refuse in the celestial careless slag behind the celestial herb rubber and abandon, cause the huge wasting of resources.Lack systematic research to extracting Quercetin at present from celestial grass.

Summary of the invention:

The purpose of this invention is to provide a kind of simple, low cost, high yield, suitable industrial a kind of from the careless herb of celestial being the method for extraction separation Quercetin.

Purpose of the present invention is achieved through the following technical solutions.

A kind of from the careless herb of celestial being the method for extraction separation Quercetin, it is characterized in that: this method is as follows:

1) extracts

1. it is some to get celestial careless herb, adds about 20 times of water gagings, boils extraction, under agitation slowly add liming to pH be 8～9, add 3% boric acid then, under this pH condition, boiled 20～30 minutes;

2. filtered while hot, residue be filtration under diminished pressure 3 times repeatedly, merging filtrate, and under 60～70 degrees celsius, with concentrated hydrochloric acid amalgamation liquid being transferred to pH is 5, acid liquid was placed 24 hours, suction filtration;

3. water is washed till neutrality with throw out, and the dry rutin crude product that gets of 60 degree is used the boiling water recrystallization, 70～80 degrees centigrade of pure product of dried rutin;

4. refining rutin to add 2%H at 1: 80 ₂SO ₄, fire heating 2h cools off suction filtration again;

5. the residual assorted neutrality that is washed to, 95% ethyl alcohol recrystallization, dextran gel column chromatography separate (SphadexLH20) then, make eluent with methyl alcohol;

6. can not be because of rutin by wash-out, thus the yellowish green colour purity product of Quercetin obtained;

2) differentiate

1. adopt the Quercetin in the tlc evaluation flavonol compound, the silica gel G plate launches with toluene-ethyl acetate-formic acid (5: 4: 1); The check of 3% aluminum chloride ethanol liquid, ultraviolet lamp (365nm) is observed; Through expansion, colour developing, show the spot of Quercetin, Rf value=0.58, refining Quercetin and standard substance are at corresponding position difference displaing yellow spot;

2. adopt the high performance liquid chromatograph method to differentiate the content of measuring Quercetin in the flavonol compound, chromatographic column: Ultimate XB-C ₁₈(5um, 4.6mm * 250mm), moving phase: acetonitrile-0.4% phosphoric acid (45: 55), flow velocity: 1.0mlmin ^-1, detect wavelength: 360nm, column temperature: 25 ℃; Extract crystallization as a result the chromatographic peak similar to the standard Quercetin occurred at 11.58 minutes, proved that the gained crystal is a Quercetin; Through formulating the standard substance curve, recording extract crystalline quercetin content is 96.8%.

The present invention compared with prior art has the following advantages.

The present invention is raw materials used cheap and easy to get, and environment is not produced pollution substantially, and simple for process, quick, the Quercetin cost that is obtained is lower, purity is high, so be fit to industrial scale production.

Embodiment

Below the present invention is described in further detail.

Of the present invention from the careless herb of celestial being the concrete steps of the method for extraction separation Quercetin be:

A kind of from the careless herb of celestial being the method for extraction separation Quercetin, it is characterized in that: this method is as follows:

1) extracts

1. it is some to get celestial careless herb, adds about 20 times of water gagings, boils extraction, under agitation slowly add liming to pH be 8～9, add 3% boric acid then, under this pH condition, boiled 20～30 minutes;

2. filtered while hot, residue be filtration under diminished pressure 3 times repeatedly, merging filtrate, and under 60～70 degrees celsius, with concentrated hydrochloric acid amalgamation liquid being transferred to pH is 5, acid liquid was placed 24 hours, suction filtration;

3. water is washed till neutrality with throw out, and the dry rutin crude product that gets of 60 degree is used the boiling water recrystallization, 70～80 degrees centigrade of pure product of dried rutin;

4. refining rutin to add 2%H at 1: 80 ₂SO ₄, fire heating 2h cools off suction filtration again;

5. the residual assorted neutrality that is washed to is separated (SphadexLH20) with 95% ethyl alcohol recrystallization, dextran gel column chromatography then, makees eluent with methyl alcohol;

6. can not be because of rutin by wash-out, thus the yellowish green colour purity product of Quercetin obtained;

2) differentiate

1. adopt the Quercetin in the tlc evaluation flavonol compound, the silica gel G plate launches with toluene-ethyl acetate-formic acid (5: 4: 1); The check of 3% aluminum chloride ethanol liquid, ultraviolet lamp (365nm) is observed; Through expansion, colour developing, show the spot of Quercetin, Rf value=0.58, refining Quercetin and standard substance are at corresponding position difference displaing yellow spot;

2. adopt the high performance liquid chromatograph method to differentiate the content of measuring Quercetin in the flavonol compound, chromatographic column: Ultimate XB-C ₁₈(5um, 4.6mm * 250mm), moving phase: acetonitrile-0.4% phosphoric acid (45: 55), flow velocity: 1.0mlmin ^-1, detect wavelength: 360nm, column temperature: 25 ℃; Extract crystallization as a result the chromatographic peak similar to the standard Quercetin occurred at 11.58 minutes, proved that the gained crystal is a Quercetin; Through formulating the standard substance curve, recording extract crystalline quercetin content is 96.8%.

Claims (1)

1. the method for an extraction separation Quercetin from the careless herb of celestial being, it is characterized in that: this method is as follows:

1) extracts

1. it is some to get celestial careless herb, adds about 20 times of water gagings, boils extraction, under agitation slowly add liming to pH be 8～9, add 3% boric acid then, under this pH condition, boiled 20～30 minutes;

2. filtered while hot, residue be filtration under diminished pressure 3 times repeatedly, merging filtrate, and under 60～70 degrees celsius, with concentrated hydrochloric acid amalgamation liquid being transferred to pH is 5, acid liquid was placed 24 hours, suction filtration;

3. water is washed till neutrality with throw out, and the dry rutin crude product that gets of 60 degree is used the boiling water recrystallization, gets the pure product of rutin after 70～80 degrees centigrade of dryings;

4. refining rutin to add 2%H at 1: 80 ₂SO ₄, fire heating 2h cools off suction filtration again;

5. the residual assorted neutrality that is washed to, 95% ethyl alcohol recrystallization, dextran gel column chromatography separate (SphadexLH20) then, make eluent with methyl alcohol;

6. can not be because of rutin by wash-out, thus the yellowish green colour purity product of Quercetin obtained;

2) differentiate

1. adopt the Quercetin in the tlc evaluation flavonol compound, the silica gel G plate launches with toluene-ethyl acetate-formic acid (5: 4: 1); The check of 3% aluminum chloride ethanol liquid, ultraviolet lamp (365nm) is observed; Through expansion, colour developing, show the spot of Quercetin, Rf value=0.58, refining Quercetin and standard substance are at corresponding position difference displaing yellow spot;

2. adopt the high performance liquid chromatograph method to differentiate the content of measuring Quercetin in the flavonol compound, chromatographic column: Ultimate XB-C ₁₈(5um, 4.6mm * 250mm), moving phase: acetonitrile-0.4% phosphoric acid (45: 55), flow velocity: 1.0mlmin ^-1, detect wavelength: 360nm, column temperature: 25 ℃; Extract crystallization as a result the chromatographic peak similar to the standard Quercetin occurred at 11.58 minutes, proved that the gained crystal is a Quercetin; Through formulating the standard substance curve, recording extract crystalline quercetin content is 96.8%.