CN102349937B - Preparation method of ixeris sonchifolia hance extractive - Google Patents
Preparation method of ixeris sonchifolia hance extractive Download PDFInfo
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- CN102349937B CN102349937B CN 201110325976 CN201110325976A CN102349937B CN 102349937 B CN102349937 B CN 102349937B CN 201110325976 CN201110325976 CN 201110325976 CN 201110325976 A CN201110325976 A CN 201110325976A CN 102349937 B CN102349937 B CN 102349937B
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Abstract
The invention discloses a preparation method for reserving ixeris sonchifolia hance extractive effective constituent, belonging to ixeris sonchifolia extraction field and aiming at solving the technical problems of the conventional preparation method of the ixeris sonchifolia hance extractive that the process is complex and organic acid is almost drained or damaged by lime cream. The preparation method includes the following stages: first, decocting the ixeris sonchifolia hance through deionized water twice and concentrating into clear paste; second, adding water to the clear paste to adjust the pH value, standing, collecting liquid supernatant, adjusting the pH value to 2-3, standing and then collecting the liquid supernatant; third, passing the liquid supernatant collected in stage 2 through a polyamide resin column, eluting with deionized water, eluting with ethanol solution to get rid of the resin column after pouring out the eluting water, and collecting the ethanol eluent; and fourth, distilling the ethanol eluent under reduced pressure to recover the ethanol, adjusting the pH value to 6.0-7.0, concentrating and drying under reduced pressure. In this way, the ixeris sonchifolia hance extractive can be obtained. Through the preparation method disclosed by the invention, the yield of the extractive can exceed 2.0% and the content of total flavonoids contained in the extractive is over 80%.
Description
Technical field
The invention belongs to sowthistle-leaf ixeris seedling and extract the field; Be specifically related to the preparation method of ixeri sonhifolia extract.
Background technology
Irexis sonchifolia [Ixeris sonchifolia (Bge.) Hance] is composite family (Compositae) gutweed Lepidium (Ixeris genus) plant, another name is sowthistle-leaf ixeris seedling, magnitude all over the sky, record in " Drug Standard of Ministry of Public Health of the Peoples Republic of China-anaesthetic fascicle " 25 pages, abound with in China northeast, North China and other places." Inner Mongol Chinese herbal medicine " record, irexis sonchifolia bitter, suffering, tool is clearing heat and detoxicating, the effect of toxin expelling, pain relieving.Among the peoplely be mainly used in treating the diseases such as appendicitis, tonsillitis, nameless gall.Whole world denticulate ixeris herb platymiscium has more than 50 and plants, and mainly is distributed in the ground such as China, Korea, Japan, Vietnam and the former Soviet Union.The total denticulate ixeris herb platymiscium more than 20 of China is planted.In recent years, along with the develop rapidly that the modern times are extracted separation and Wave Spectrum technology and modern pharmacology, more and more deep to chemical composition and the bioactive research of denticulate ixeris herb platymiscium.Through chemical analysis, its Main Ingredients and Appearance is flavonoids, phenolic acid class and sesquiterpene lactone class, triterpene substance, is the material base of its performance pharmacologically active.Modern pharmacological research confirms that the ixeris sonchifolia hance extract pharmacological action is comparatively extensive: the ⑴ heart, cerebrovascular protective effect; Have the increase coronary flow, reduce oxygen metabolism, improve hypoxia-bearing capability, to the therapeutic action of experimental myocardial infarction, increase cerebral blood flow (CBF), improve microcirculation, the vasoconstriction effect.⑵ to the effect of hematological system; Has platelet aggregation-against, fortifying fibre proteinase activity, reducing blood lipid, promoting blood circulation and removing blood stasis, study of anti-atherogenic effect.⑶ analgesia, sedation; ⑷ anti-oxidant and effect of scavenging radical; ⑸ antitumor action; ⑹ preventing respiratory viruses effect; ⑺ liver protection; ⑻ other effects; Such as membrane stabilizing action, improve the protective effect of ability of learning and memory, acute injury of kidney etc.Therefore, study now more denticulate ixeris herb general flavone and total phenolic acid and have great clinical value and market development value as the medical active position.
General flavone content is with anhydrous rutin (C in the ixeri sonhifolia extract that the inventive method obtains
27H
30O
16) meter, be no less than 80%; Monomer component cyanidenon (C
15H
10O
6) content is no less than 7.0%.Also contain caffeic acid, galuteolin, cyanidenon glucuronic acid glycosides, Cichoric acid, sodium element etc.
The preparation method of ixeri sonhifolia extract is a lot, but be applied to the industrial stone sulphur method that only has, the method is mainly in flavones ingredient, and other compositions such as organic acids basically run off or destroyed by milk of lime, in extract, produce simultaneously the residual of calcium salt, bring certain potential safety hazard.Other method is laboratory procedure basically, for example adopts the silicagel column separation and purification; Organic solvent (such as, ethyl acetate, n-butanol) extraction etc.So that performance difficulty in suitability for industrialized production, or can not implement at all.Though ZL 200410078168.0 disclosed methods have adopted the polyamide purifying means, also adopted simultaneously the shitosan precipitation, adopted again alcohol precipitation for removing glycan, simultaneously for improving general flavone content, adopt again 90% acetone treatment, so that complex process, the low industrialization operation requirements condition of acetone boiling point is higher simultaneously.
Wherein, " research and development of natural products " (2010.22:430-432) in disclosed article " separation of irexis sonchifolia water soluble ingredient and Structural Identification ", employing calcium oxide precipitation liquid is disclosed, and adopt NaOH to regulate liquid to neutral, adopting the ethanol precipitation, after polyamide column, although the method has solved the problem of removing the large molecular impurities such as tannin, but without any improvement, and the step of removal of impurities is more, has aggravated the loss of active ingredient to the reservation of active ingredient.
Summary of the invention
The present invention will solve the technical problem that existing ixeri sonhifolia extract preparation method exists complex process, organic acid basically to run off or destroyed by milk of lime; And provide a kind of preparation method that can keep ixeri sonhifolia extract active ingredient.
The preparation method of ixeri sonhifolia extract carries out in the steps below among the present invention: step 1, get 100kg irexis sonchifolia Chinese medicine, then decoct 2 times with deionized water, the quality that decocts for the first time deionized water is 16～20 times of irexis sonchifolia Chinese medicine, the consumption that decocts for the second time deionized water is 12～16 times of irexis sonchifolia Chinese medicine quality, the each decoction 1 hour consuming time, merge decoction liquor twice, be concentrated into again take the clear cream of 80 ℃ of relative densities as 1.12～1.16; Add water in step 2, the clear cream with the step 1 acquisition, adding water to volume is 200L, then be 10% sodium hydroxide solution adjust pH to 6.5～7.0 with mass concentration, left standstill 12～24 hours, collect supernatant, then supernatant left standstill 12～24 hours with hydrochloric acid solution adjust pH to 2～3, collected supernatant liquid; Step 3, the supernatant liquid that step 2 is collected are crossed polyamide resin column, the mass ratio of crossing polyamide quality and medicinal material (irexis sonchifolia) is 1:2.25, carry out wash-out with deionized water again, the deionized water volume that wash-out is used is 6～10 column volumes, it is 55%～85% ethanolic solution wash-out resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that wash-out is used is 5 column volumes, collects ethanol eluate; Step 4, ethanol eluate is carried out the decompression distillation Recycled ethanol, with sodium hydroxide solution adjust pH 6.0～7.0, concentrated, drying under reduced pressure namely obtains ixeri sonhifolia extract.
Adopt the method for acid treatment extract to remove the larger tannin class material of molecular weight, use polyamide to process, adopt 80% ethanol elution, this technique is further removed macromolecular albumen, tannin and resinae material.So that the Flavonoid substances of enrichment molecular weight and organic phenol acid substance.The key point of this invention is to adopt before polyamide processes, and adopts first the acid treatment extract, and flavones and organic acid in the extract are all entered in the resin column under the non-salification, and can be more completely by resin adsorption, and specific aim is better.Adopt simultaneously 80% ethanol more completely desorb flavones and organic acid.This technique is except ethanol, do not use other organic solvents, so that technological process is simple, production equipment requires lower, manufacturing cost reduces, simultaneously the method extract yield highlyer surpass 2.0%, this extractive total flavone content surpasses 80%, reach the specification requirement of national traditional Chinese medicine raw material, this extract can be used as the raw material of traditional Chinese medicine raw material or oral formulations.
Description of drawings
Fig. 1 is ixeri sonhifolia extract HPLC spectrogram.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the preparation method of ixeri sonhifolia extract carries out in the steps below in the present embodiment:
Step 1, get 100kg irexis sonchifolia Chinese medicine, then decoct 2 times with deionized water, the quality that decocts for the first time deionized water is 16～20 times of irexis sonchifolia Chinese medicine, the consumption that decocts for the second time deionized water is 12～16 times of irexis sonchifolia Chinese medicine quality, the each decoction 1 hour consuming time, merge decoction liquor twice, be concentrated into again take the clear cream of 80 ℃ of relative densities as 1.12～1.16;
Add water in step 2, the clear cream with the step 1 acquisition, adding water to volume is 200L, then be 10% sodium hydroxide solution adjust pH to 6.5～7.0 with mass concentration, left standstill 12～24 hours, collect supernatant, then supernatant left standstill 12～24 hours with hydrochloric acid solution adjust pH to 2～3, collected supernatant liquid;
Step 3, the supernatant liquid that step 2 is collected are crossed polyamide resin column, the mass ratio of crossing polyamide and medicinal material (irexis sonchifolia medicinal material) is 1:2.25, carry out wash-out with deionized water again, the deionized water volume that wash-out is used is 6～10 column volumes, it is 55%～85% ethanolic solution wash-out resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that wash-out is used is 5 column volumes, collects ethanol eluate;
Step 4, ethanol eluate is carried out the decompression distillation Recycled ethanol, with sodium hydroxide solution adjust pH 6.0～7.0, concentrated, drying under reduced pressure namely obtains ixeri sonhifolia extract.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the mass concentration of the described hydrochloric acid solution of step 2 is 5%.Other step is identical with implementation one with parameter.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is: the volumetric concentration of the described ethanolic solution of step 3 is 60%～80%.Other step is identical with implementation one or two with parameter.
The specific embodiment four: what present embodiment was different from the specific embodiment one or two is: the volumetric concentration of the described ethanolic solution of step 3 is 80%.Other step is identical with implementation one or two with parameter.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to four is: the mass concentration of sodium hydroxide solution described in the step 4 is 10%.Other step is identical with one of specific embodiment one to four with parameter.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is: described drying under reduced pressure temperature is 60～80 ℃, and the drying under reduced pressure time is 6～10 hours.Other step is identical with one of specific embodiment one to five with parameter.
Adopt following verification experimental verification invention effect:
Test one: the preparation method of ixeri sonhifolia extract carries out in the steps below in the present embodiment: get irexis sonchifolia medicinal material 100kg, adding deionized water decocts 2 times, amount of water is respectively 20 times, 16 times of medicinal material amount, decocting time was respectively 1.0 hours, collecting decoction is concentrated into relative density 1.12～1.16(80 ℃) clear cream; Clear cream adds water to a times of crude drug amount, and adjust pH 6.5～7.0 left standstill 24 hours, collects supernatant, and precipitation discards; Supernatant left standstill 24 hours with 5% hydrochloric acid adjust pH 2.0～3.0, collected supernatant and crossed the polyamide resin column of having handled well, and the resin medicinal material is than w/w(1:2.25), wash 6～10 column volumes, use again 5 column volumes of 80% ethanol elution, collect alcohol eluen; Recycled ethanol, liquid is with 10% sodium hydroxide solution adjust pH to 6.5～7.0, and is concentrated, drying under reduced pressure, extract yield 〉=2.2%.
Main component is flavones, organic acid in the extract; It is the flavones of parent nucleus that flavones has cyanidenon, and galuteolin, cyanidenon-7-O-β-D-Glucose aldehydic acid glycosides, organic acid mainly are caffeoyl series organic acids, comprise caffeic acid, Cichoric acid etc.
The component case study result of this extract
General flavone content is with anhydrous rutin (C in the extract
27H
30O
16) meter, be no less than 80%; Monomer component cyanidenon (C
15H
10O
6) content is no less than 7.0%, its constituent: cyanidenon-7-O-β-D-Glucose aldehydic acid glycosides C
21H
17O
12) content is no less than 9.0%; Galuteolin (C
21H
20O
11) content is no less than 0.7%; Cichoric acid (C
22H
18O
12) content be no less than 5.5%; Caffeic acid (C
9H
8O
4) content be no less than 0.6%; Sodium ions content is more than 7.5%.
The pilot study of 6 main components
1 material, reagent and reagent
High performance liquid chromatograph Agilent 1100 series liquid chromatograph instrument are furnished with online degasser; Quaternary gradient elution pump; Column oven
Galuteolin chemical reference substance lot number: 111720-200501
Caffeic acid chemical reference substance lot number: 110885-200102
Rutin chemical reference substance lot number: 110080-200306
Cyanidenon chemical reference substance lot number: 111520-200504
Provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Cyanidenon-7-O-glucuronic acid glycosides is provided by crude drug teaching and research room of Shenyang Pharmaceutical University
Cichoric acid provides (99.1%byHPLC) by U.S. SIGMA-ALDRICH
Chromatographic column Penomenex
Luna C18 250 * 4.6mm 5 μ m
Reagent methyl alcohol, acetonitrile chromatographically pure (DIKMA)
Other reagent of sodium chloride standard reagent is that commercially available analysis is pure
The reagent ixeri sonhifolia extract is provided by No. 2 TCM Factory
Lot number: 070201,070501,060601,080701
2 test methods and result
2.1 test method
The determined by ultraviolet spectrophotometry general flavone is adopted in the ixeri sonhifolia extract quality control, adopts acid hydrolysis, Syrups by HPLC flavone aglycone cyanidenon.
Large constituents in the ixeri sonhifolia extract mainly is organic acid and flavonoids composition, by document and standard items location, tentatively think and contain caffeic acid, galuteolin, cyanidenon glucuronide, four kinds of compositions of Cichoric acid in the ixeri sonhifolia extract, all adopt high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D) to carry out assay.Be filler with octadecylsilane chemically bonded silica; Acetonitrile-water-phosphoric acid system is mobile phase; Detect wavelength: organic acid is that 324nm, flavones ingredient are 350nm; Owing in preparation technology, used NaOH to regulate acid-base value, simultaneously the sodium element in the finished product is carried out assay, sodium element adopts the flame method atomic absorption spectroscopy determination.
2.2 result of the test
2-1 ixeri sonhifolia extract quality control assay result
By the known composition of part is carried out assay, its content results 2-1 that sees the following form
The known component content result of study of table 2-2 ixeri sonhifolia extract
Ixeri sonhifolia extract quality control index composition, general flavone content is with anhydrous rutin (C
27H
30O
16) meter, be no less than 80%; Monomer component cyanidenon (C
15H
10O
6) content is no less than 7.0%.
By high-efficient liquid phase technique to the known composition pilot study of part, the (see figure 1) of clear and definite structure has caffeic acid (tR=4.886min), galuteolin (tR=7.610min), cyanidenon glucuronic acid glycosides (tR=8.142min), Cichoric acid (tR=9.398min), five kinds of compositions of sodium metal element in the ixeri sonhifolia extract, and five kinds of compositions have been carried out assay, wherein caffeic acid 0.94%; Galuteolin 0.79%; Cyanidenon glucuronic acid glycosides 10.65%; Cichoric acid 6.16%; Sodium element 7.76%.Each component content is more stable, and Primary Study confirms that the controlled composition in the extract reaches about 25%.
Claims (6)
1. preparation method that can keep ixeri sonhifolia extract active ingredient is characterized in that the preparation method that can keep ixeri sonhifolia extract active ingredient carries out in the steps below:
Step 1, get 100kg irexis sonchifolia Chinese medicine, then decoct 2 times with deionized water, the quality that decocts for the first time deionized water is 16～20 times of irexis sonchifolia Chinese medicine, the consumption that decocts for the second time deionized water is 12～16 times of irexis sonchifolia Chinese medicine quality, the each decoction 1 hour consuming time, merge decoction liquor twice, be concentrated into again take the clear cream of 80 ℃ of relative densities as 1.12～1.16;
Add water in step 2, the clear cream with the step 1 acquisition, adding water to volume is 200L, then be 10% sodium hydroxide solution adjust pH to 6.5～7.0 with mass concentration, left standstill 12～24 hours, collect supernatant, then supernatant left standstill 12～24 hours with hydrochloric acid solution adjust pH to 2～3, collected supernatant liquid;
Step 3, the supernatant liquid that step 2 is collected are crossed polyamide resin column, the mass ratio of polyamide and irexis sonchifolia is 1:2.25, carry out wash-out with deionized water again, the deionized water volume that wash-out is used is 6～10 column volumes, it is 55%～85% ethanolic solution wash-out resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that wash-out is used is 5 column volumes, collects ethanol eluate;
Step 4, ethanol eluate is carried out the decompression distillation Recycled ethanol, with sodium hydroxide solution adjust pH 6.0～7.0, concentrated, drying under reduced pressure namely obtains ixeri sonhifolia extract.
2. a kind of preparation method that can keep ixeri sonhifolia extract active ingredient according to claim 1, the mass concentration that it is characterized in that the described hydrochloric acid solution of step 2 is 5%.
3. a kind of preparation method that can keep ixeri sonhifolia extract active ingredient according to claim 2, the volumetric concentration that it is characterized in that the described ethanolic solution of step 3 is 60%～80%.
4. a kind of preparation method that can keep ixeri sonhifolia extract active ingredient according to claim 2, the volumetric concentration that it is characterized in that the described ethanolic solution of step 3 is 80%.
5. the described a kind of preparation method that can keep ixeri sonhifolia extract active ingredient of each claim according to claim 1-4, the mass concentration that it is characterized in that sodium hydroxide solution described in the step 4 is 10%.
6. the described a kind of preparation method that can keep ixeri sonhifolia extract active ingredient of each claim according to claim 5 is characterized in that described drying under reduced pressure temperature is 60～80 ℃, and the drying under reduced pressure time is 6～10 hours.
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Effective date of registration: 20211217 Address after: 150000 room a307-169, building 20, innovation and entrepreneurship Plaza, science and technology innovation city, high tech Industrial Development Zone, Harbin, Heilongjiang Province (178 Xiuyue Street) Patentee after: Harbin Pharmaceutical Group traditional Chinese Medicine Co.,Ltd. Address before: 150078 No. 243 Airport Road, Daoli District, Heilongjiang, Harbin Patentee before: The Second Chinese Medicine Factory, Harbin Pharmaceutical Group Co.,Ltd. |