CN102813686B - Method for extracting active ingredients from hibiscus sabdariffa calyx - Google Patents
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Abstract
The present invention relates to a method for extracting active ingredients from hibiscus sabdariffa calyx, and belongs to the technical field of extraction of active ingredients from hibiscus sabdariffa. The extraction process comprises: crushing dried hibiscus sabdariffa calyx; filling the crushed calyx in a reaction kettle liner of a subcritical water extraction tank; adding water with a pH value of 1.0-3.0 according to a liquid-solid ratio of 15:1-25:1, wherein an extraction pressure is 5-10 MPa, an extraction temperature is 110-150 DEG C, and an extraction time is 20-50 min; filtering; carrying out reduced pressure concentration on the resulting filtrate to a dry state; adding water to dissolve; and carrying out freeze drying to obtain the active ingredient extract of the hibiscus sabdariffa calyx. Compared with the traditional water extraction method and the 30% ethanol extraction method, the method of the present invention has advantages of short extraction time, high extract yield, green environment protection, and no pollution.
Description
Technical field
The present invention relates to a kind of new method and technique of extracting effective ingredient in Calyx Hibisci Sabdariffae, refer in particular to the Method and process that adopts subcritical water to extract effective ingredient in Calyx Hibisci Sabdariffae.
Background technology
Calyx Hibisci Sabdariffae (
hibiscus sabdariffa. L) have another name called Hibiscus Sabdariffa Linn, roselle, red sorrel etc., Malvaceae Hibiscus annual herb plant or perennial shrub, be traditional medicine food dual purpose plant.Calyx Hibisci Sabdariffae grows in subtropical and tropical zones, originates in West Africa, India and Malaysia, and the plantation history of existing centuries is so far imported Taiwan plantation for 1910 into, nowadays equal establishing in large scale in China Guangdong, Guangxi, Fujian, Taiwan, Yunnan.Traditional medicine thinks, Calyx Hibisci Sabdariffae has heat clearing away, quench one's thirst and effect of blood pressure lowering, and modern medicine study proves, Calyx Hibisci Sabdariffae has antioxidation, antitumor, antibacterial and improve the pharmacological actions such as atheroma.In Calyx Hibisci Sabdariffae, contain the various active compositions such as aminoacid, organic acid, polysaccharide, vitamin, anthocyanin, phenols, wherein main effective ingredient is anthocyanin and polyphenols.
Subcritical water (Subcritical Water), refer to higher than 100 ℃ lower than the critical pressure (Pc=22.1 MPa) of water and the aqueous water of critical temperature (Tc=374 ℃), because of temperature higher, polarity, surface tension and the viscosity of subcritical water all sharply declines, solvability to middle polarity and low pole compound increases greatly, and its character is closer to organic solvent.Subcritical water extractive technique is to utilize subcritical water as the novel extraction and separation technology of one that extracts solvent, this technology has short, the technical advantage such as extraction yield is high, environmental friendliness of extraction time, be a kind of green extractive technique that is easy to realize suitability for industrialized production, therefore in natural drug extracts active ingredients separation application, development prospect is wide.
The large more options ethanol of extraction solvent of effective ingredient in Calyx Hibisci Sabdariffae at present, extracting method, except conventional heat is extracted, has (grain and oils and fats, 2010, (11): 40-43) such as ultrasonic assisted extraction, microwave-assisted extraction, membrane technology extractions.Li Shengfeng etc. are take 40% ethanol as solvent, and temperature is 75 ℃, and the time is within 1.5 hours, to extract antioxidant polyphenol and the anthocyanidin in Calyx Hibisci Sabdariffae, total polyphenols extraction efficiency is 0.975%, anthocyanidin extraction efficiency is 0.074%(hubei agricultural science, 2007,46(1) 133-135).The reports such as figure Zong Cai adopt anthocyanidin in ultrasound wave assisted extraction Calyx Hibisci Sabdariffae, at solid-to-liquid ratio 1: 25(g/mL), extract 50 ℃ of temperature, extraction times 20 min, under the optimum process condition of ultrasonic power 80 W, anthocyanidin yield is 0.566%, compares than traditional extraction, yield has improved 14.3 %, and shorten extraction time (food research and development, 2011,32(10): 1-4).Patent of invention (application number 201010507916.8) discloses the method for red pigment in a kind of hot water extraction Calyx Hibisci Sabdariffae, liquid-solid ratio is 20:1, heating in water bath filters to insulation 30-40 min after boiling, extracts three times, is evaporated to solids content and is 30 ~ 40% roselle calyx red pigment extractum.But about adopt subcritical water to extract the method for effective ingredient in Calyx Hibisci Sabdariffae so far there are no report both at home and abroad, also have no corresponding patent open.
Summary of the invention
The object of the invention is the deficiency existing in above-mentioned background technology for solving, a kind of new method and technique of extracting effective ingredient in Calyx Hibisci Sabdariffae is provided.
For foregoing invention object, the present invention adopts following technical scheme: dry Calyx Hibisci Sabdariffae after crushed, get the reactor inner bag that certain mass powder is placed in subcritical water extraction pot, add the water of appropriate certain pH value, under certain extraction pressure and temperature, extract certain hour, filter, filtrate decompression is concentrated into dry, the postlyophilization that is dissolved in water, obtains Calyx Hibisci Sabdariffae effective component extracts.
Concrete extraction process is: a kind of method of extracting effective ingredient in Calyx Hibisci Sabdariffae, carry out according to following step:
Dry Calyx Hibisci Sabdariffae is pulverized, pack in the reactor inner bag of subcritical water extraction pot, adding pH value by liquid-solid ratio 15:1 ~ 25:1 is 1.0 ~ 3.0 water, extracting pressure is 5 ~ 10 MPa, and extracting temperature is 110 ~ 150 ℃, extraction times 20 ~ 50 min, filter, gained filtrate decompression is concentrated into dry, and the postlyophilization that is dissolved in water obtains Calyx Hibisci Sabdariffae effective component extracts.
This Calyx Hibisci Sabdariffae effective component extracts yield is 46.4 ~ 63.4 %, and in extract, anthocyanin content is 0.13 ~ 0.28 mg/g, and polyphenol content is 13.0 ~ 13.3 mg/g.
Compared with prior art, its remarkable advantage is that extraction time is short, extract yield is high, green non-pollution in the present invention.Take Calyx Hibisci Sabdariffae dry flower calyx as raw material, adopt subcritical water extraction method to extract effective ingredient wherein, yield can reach 63.4%, and once extract yield than traditional water extraction and improved 61.3%, and higher than traditional water extraction extracted twice yield; Once extract yield than 30% ethanol extraction method and improved 46.7%, higher than extracted twice yield.Adopt subcritical water extraction method, when liquid-solid ratio is 20:1, pH is 1.5, and extracting pressure is 7 MPa, and extracting temperature is 130 ℃, and extraction time, while being 40 min, in extract, active constituent content was apparently higher than traditional water extraction and 30% ethanol extraction method.Antioxidant activity is tested and is shown, under this condition, subcritical water extract antioxidant activity and 30% ethanol extraction is close, higher than the antioxidant activity of traditional water extract.
accompanying drawing explanation
Wherein Fig. 1 is the removing ability of Calyx Hibisci Sabdariffae extract to DPPH free radical, note: SWE: subcritical water extract; ERE30%:30% ethanol extraction; HWE: traditional water extract.
the specific embodiment:
In order to be illustrated more clearly in content of the present invention, be described as follows with specific embodiment, specific embodiment does not limit context of the present invention.
the preparation of Calyx Hibisci Sabdariffae effective component extracts
comparative example 1:
Take Calyx Hibisci Sabdariffae dry flower calyx powder 2.5000 g, by liquid-solid ratio 20:1(v/w, mL/g) add 50.00 mL water, with hydrochloric acid tune pH to 1.5, in the water-bath of 75 ℃, extract 1h, extract twice, twice filtrate and be evaporated to respectively dry, add suitable quantity of water and dissolve postlyophilization, obtain Calyx Hibisci Sabdariffae extract.Extract weighs 0.9825 g for the first time, and extracting yield is 39.3%, and wherein anthocyanin content is 0.18 mg/g, and polyphenol content is 9.2 mg/g; Extract weighs 0.1250 g for the second time, and extracting yield is 5.0%, and wherein anthocyanin content is 0.14 mg/g, and polyphenol content is 9.9 mg/g.Extracted twice thing gross weight 1.1075g, total yield is 44.3%, and anthocyanin content is 0.18 mg/g, and polyphenol content is 9.3 mg/g.
comparative example 2:
Replace water with 30% alcoholic solution, according to comparative example 1, with method operation, extract weighs 1.0800 g for the first time, and extracting yield is 43.2%, and wherein anthocyanin content is 0.24 mg/g, and polyphenol content is 12.7 mg/g; Extract weighs 0.2050 g for the second time, and extracting yield is 8.2%, and wherein anthocyanin content is 0.18 mg/g, and polyphenol content is 12.6 mg/g.Extracted twice thing weighs 1.2850 g, and total yield is 51.4%, and anthocyanin content is 0.23 mg/g, and polyphenol content is 12.7 mg/g.
embodiment 1:
Get Calyx Hibisci Sabdariffae dry flower calyx powder 2.5000 g, be placed in the inner bag of subcritical water extraction pot reactor, by liquid-solid ratio 15:1(v/w, mL/g) add the water that 37.50 mL pH value are 1.0, extracting pressure is 5 MPa, extracting temperature is 110 ℃, extraction time is 20 min, filter, concentrate filtrate to dryly, postlyophilization is dissolved in water, obtain Calyx Hibisci Sabdariffae effective component extracts 1.1600 g, extracting yield is 46.4%, and in extract, anthocyanin content is 0.21 mg/g, and polyphenol content is 13.0 mg/g.
embodiment 2:
Get Calyx Hibisci Sabdariffae powder 2.5000 g, be placed in the inner bag of subcritical water extraction pot reactor, by liquid-solid ratio 20:1(v/w, mL/g) add the water that 50.00 mL pH value are 1.5, extracting pressure is 7 MPa, extracting temperature is 130 ℃, and extraction times 40 min filters, filtrate decompression is concentrated into dry, the postlyophilization that is dissolved in water, obtains Calyx Hibisci Sabdariffae effective component extracts 1.5850 g, and extracting yield is 63.4%.In extract, anthocyanin content is 0.28 mg/g, and polyphenol content is 13.3 mg/g.
embodiment 3:
Get Calyx Hibisci Sabdariffae dry flower calyx powder 2.5000 g, be placed in the inner bag of subcritical water extraction pot reactor, by liquid-solid ratio 25:1(v/w, mL/g) add the water that 62.50 mL pH value are 3.0, extracting pressure is 10 MPa, extracting temperature is 150 ℃, and extraction times 50 min filters, concentrate filtrate to dry, the postlyophilization that is dissolved in water, obtains Calyx Hibisci Sabdariffae effective component extracts 1.5750 g, and extracting yield is 63.0%.In extract, anthocyanin content is 0.13 mg/g, and polyphenol content is 13.3 mg/g.
calyx Hibisci Sabdariffae effective component extracts Antioxidative Activity Determination
embodiment 4 Calyx Hibisci Sabdariffae effective component extracts are removed DPPH Free Radical
Investigate the antioxidant activity of given the test agent by removing the test of DPPH free radical.
1, experiment material
1.1 medicines and reagent
The extract of Calyx Hibisci Sabdariffae extract: embodiment 2, the aqueous solution that is mixed with crude drug concentration 2 mg/mL is for subsequent use
DPPH(1,1-diphenyl picryl phenylhydrazine) purchased from Sigma company
1.2 instruments:
TU1800 ultraviolet-visible spectrophotometer, Beijing is general analyses the reduction of fractions to a common denominator and analyses instrument plant
BS124S electronic balance: Beijing Sai Duolisi instrument system company limited;
2,
experimental technique
The preparation of 2.1 DPPH alcoholic solution
Accurately take 7.9 mg DPPH standard substance, dissolve and be settled in the brown volumetric flask of 100 mL with ethanol solution, be made into the DPPH alcoholic solution of 0.2 mmol/L, be placed in 4 ℃ of refrigerators and preserve, for subsequent use.
2.2 assay method
Measure respectively 2 mL sample solutions in test tube, add the DPPH alcoholic solution of 2 mL, after mix homogeneously, 30 min are reacted in dark place, then measure its absorbance (A in 517 nm places
i), replace sample solution to measure blank absorbency (A with sample solvent
0), replace DPPH measured in solution absorbance (A with dehydrated alcohol
j), clearance rate computing formula is as follows:
3, experimental result
Accompanying drawing is the removing ability of Calyx Hibisci Sabdariffae extract to DPPH free radical.As shown in Figure 1, Calyx Hibisci Sabdariffae subcritical water extract has good removing ability to DPPH free radical, in the time that extract concentrations is 1mg/mL, to the removing Li Keda 86.1% of DPPH free radical, Vc, subcritical water extract (SWE), 30% ethanol extraction (ERE30%) and the IC of traditional water extract (HWE) to DPPH free radical scavenging
50be respectively 12,582,528 and 798 μ g/mL.The removing ability of visible subcritical water extract to DPPH free radical and 30% ethanol extraction close, higher than the antioxidant activity of traditional water extract.
4, conclusion
The subcritical water extract of Calyx Hibisci Sabdariffae is good to the removing ability of DPPH free radical, and its removing ability and 30% ethanol extraction close, higher than the antioxidant activity of traditional water extract.
Claims (1)
1. extract a method for effective ingredient in Calyx Hibisci Sabdariffae, it is characterized in that carrying out according to following step:
Dry Calyx Hibisci Sabdariffae is pulverized, pack in the reactor inner bag of subcritical water extraction pot, adding pH value by liquid-solid ratio 15:1 ~ 25:1 is 1.0 ~ 3.0 water, extracting pressure is 5 ~ 10 MPa, and extracting temperature is 110 ~ 150 ℃, extraction times 20 ~ 50 min, filter, gained filtrate decompression is concentrated into dry, and the postlyophilization that is dissolved in water obtains Calyx Hibisci Sabdariffae effective component extracts;
The yield of Calyx Hibisci Sabdariffae effective component extracts is 46.4 ~ 63.4 %, and in extract, anthocyanin content is 0.13 ~ 0.28 mg/g, and polyphenol content is 13.0 ~ 13.3 mg/g.
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