CN115433079A - Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation - Google Patents
Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation Download PDFInfo
- Publication number
- CN115433079A CN115433079A CN202211030884.6A CN202211030884A CN115433079A CN 115433079 A CN115433079 A CN 115433079A CN 202211030884 A CN202211030884 A CN 202211030884A CN 115433079 A CN115433079 A CN 115433079A
- Authority
- CN
- China
- Prior art keywords
- ligusticum wallichii
- irradiation
- active ingredients
- extraction efficiency
- improving
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 241000112528 Ligusticum striatum Species 0.000 title claims abstract description 154
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000000605 extraction Methods 0.000 title claims abstract description 41
- 239000004480 active ingredient Substances 0.000 title claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 56
- 238000004806 packaging method and process Methods 0.000 claims abstract description 45
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 239000006228 supernatant Substances 0.000 claims abstract description 20
- 238000002791 soaking Methods 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 17
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- 239000003795 chemical substances by application Substances 0.000 claims description 39
- 239000012528 membrane Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- 238000010894 electron beam technology Methods 0.000 claims description 11
- 231100000987 absorbed dose Toxicity 0.000 claims description 10
- 239000004677 Nylon Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 5
- 241000510667 Conioselinum Species 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000003814 drug Substances 0.000 abstract description 6
- 239000013543 active substance Substances 0.000 abstract description 5
- 230000001678 irradiating effect Effects 0.000 abstract description 3
- 238000010298 pulverizing process Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 17
- 238000002156 mixing Methods 0.000 description 15
- 238000012216 screening Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004506 ultrasonic cleaning Methods 0.000 description 10
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 9
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 description 8
- 235000001785 ferulic acid Nutrition 0.000 description 8
- 229940114124 ferulic acid Drugs 0.000 description 8
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 8
- 239000000284 extract Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- HJXMNVQARNZTEE-UHFFFAOYSA-N Butylphthalide Chemical compound C1=CC=C2C(CCCC)OC(=O)C2=C1 HJXMNVQARNZTEE-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000007605 air drying Methods 0.000 description 6
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 6
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 5
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 5
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 5
- 235000001368 chlorogenic acid Nutrition 0.000 description 5
- 229940074393 chlorogenic acid Drugs 0.000 description 5
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 5
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- IQVQXVFMNOFTMU-FLIBITNWSA-N (Z)-ligustilide Chemical compound C1CC=CC2=C1C(=C/CCC)/OC2=O IQVQXVFMNOFTMU-FLIBITNWSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- IQVQXVFMNOFTMU-DHZHZOJOSA-N Z-ligustilide Natural products C1CC=CC2=C1C(=C/CCC)\OC2=O IQVQXVFMNOFTMU-DHZHZOJOSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 241000244365 Ligusticum sinense Species 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001502 supplementing effect Effects 0.000 description 3
- 239000000341 volatile oil Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RSKPJCDZAFMWHH-UHFFFAOYSA-N 3-but-1-enyl-3h-2-benzofuran-1-one Chemical compound C1=CC=C2C(C=CCC)OC(=O)C2=C1 RSKPJCDZAFMWHH-UHFFFAOYSA-N 0.000 description 2
- AXRIHSJZHOTGAE-UHFFFAOYSA-N 3-butyl-6,7-dihydroxy-4,5,6,7-tetrahydro-3h-2-benzofuran-1-one Chemical compound C1CC(O)C(O)C2=C1C(CCCC)OC2=O AXRIHSJZHOTGAE-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- ZPIKVDODKLJKIN-NSHDSACASA-N Senkyunolide Chemical compound C1CC=CC2=C1[C@H](CCCC)OC2=O ZPIKVDODKLJKIN-NSHDSACASA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 150000002596 lactones Chemical class 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- DQNGMIQSXNGHOA-RCBCECLLSA-N (3z,6s,7r)-3-butylidene-6,7-dihydroxy-4,5,6,7-tetrahydro-2-benzofuran-1-one Chemical compound C1([C@H]([C@@H](O)CC2)O)=C2C(=C/CCC)/OC1=O DQNGMIQSXNGHOA-RCBCECLLSA-N 0.000 description 1
- 241000212948 Cnidium Species 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- DQNGMIQSXNGHOA-UHFFFAOYSA-N senkyunolide-H Natural products C1CC(O)C(O)C2=C1C(=CCCC)OC2=O DQNGMIQSXNGHOA-UHFFFAOYSA-N 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/87—Benzo [c] furans; Hydrogenated benzo [c] furans
- C07D307/88—Benzo [c] furans; Hydrogenated benzo [c] furans with one oxygen atom directly attached in position 1 or 3
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for improving the extraction efficiency of active ingredients of ligusticum wallichii by irradiation, belonging to the technical field of traditional Chinese medicine extraction and comprising the following steps: drying rhizoma Ligustici Chuanxiong, sealing in a packaging bag, and storing in dark place; irradiating the packed rhizoma Ligustici Chuanxiong with irradiation source at normal temperature and low dose; pulverizing irradiated rhizoma Ligustici Chuanxiong; adding the pulverized rhizoma Ligustici Chuanxiong into the extractant, soaking in dark place, performing ultrasonic treatment, and filtering to obtain supernatant. The ligusticum wallichii is irradiated and then extracted, so that the extraction yield of three active substances in the ligusticum wallichii is obviously improved.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, in particular to a method for improving the extraction efficiency of active ingredients of ligusticum wallichii by irradiation.
Background
The related research and development of ligusticum wallichii extraction are mainly focused at home, active substances such as essential oil, alkaloid, lactone, polysaccharide, phenols and the like are extracted from ligusticum wallichii serving as a raw material at present, methods such as water vapor extraction, carbon dioxide supercritical extraction, solvent extraction and the like are mainly adopted, and auxiliary treatment such as heating or ultrasonic treatment is usually combined.
The Chinese invention patent application (application number 200710156024.6) discloses a method for obtaining ferulic acid and 3-n-butenyl phthalide by adopting solvent heating extraction, concentration, silica gel column elution and HPLC separation, wherein the content of the ferulic acid in the extract is about 35-45%, and the content of the 3-n-butenyl phthalide is 30-40%, but the determination of other components is not related. The Chinese patent application (201710055451.9) discloses a method for preparing medicated serum from alcohol extract of Ligusticum wallichii, wherein the preparation method only relates to alcohol extract of Ligusticum wallichii comprises the steps of pulverizing Ligusticum wallichii into powder, adding ethanol for reflux extraction, freeze-drying, and pulverizing to obtain solid powder, and the process parameters of the preparation method of alcohol extract of Ligusticum wallichii are not restricted in the claims. The Chinese patent application (application No. 20211238098.0) discloses a method for extracting cnidium oil by using a water solvent, adding potassium hydrogen peroxymonosulfate composite salt into the obtained extract for reaction, and combining the steps of filtering, concentrating, extracting, chromatographic separation and the like to obtain a pure product of senkyunolide J, but the method does not relate to the extraction and separation of other components. The Chinese patent application (application No. 20211238098.0) discloses a preparation method of ligustilide extract, which mainly comprises the steps of crushing, soaking, extracting and purifying and the like to obtain the ligustilide extract, mainly containing ligustilide and senkyunolide A/H/I, but the method mainly aims at the separation and extraction of lactone components in ligusticum wallichii. The Chinese invention patent application (application number 202011459453.2) discloses a preparation method of ligusticum wallichii polysaccharide, but does not relate to the preparation of other components of ligusticum wallichii. Chinese invention patent application (application number 201910543121.3) discloses a preparation method of a traditional Chinese medicine composition with the functions of promoting blood circulation and removing blood stasis, and only describes the preparation of a crude extract of ligusticum wallichii.
Dengpeng et al (J. Pharmaceutical practice, 2020, 38 (2)) compared the difference of the main components of the volatile oil of Ligusticum wallichii extracted by supercritical CO2 extraction and steam distillation; an HPLC detection method for the main components in the epimedium-ligusticum wallichii medicament is established by Chenwenjun and the like (Chinese medicinal materials, 2020,43 (12)); zhongjunbo (J.Pharmacology, 2019, 54 (18)) through research, the extraction temperature and the crushing degree of the medicinal materials are considered as key influencing factors of the process for extracting the ligusticum wallichii volatile oil by water vapor. Chen Zhaoyu, etc. (J. Of Chinese medicine, 2021, 43 (12)) optimizes the vacuum steam moistening preparation process of rhizoma Ligustici Chuanxiong decoction pieces with ferulic acid as index, and examines the antiinflammatory and analgesic activities of rhizoma Ligustici Chuanxiong moistening decoction pieces, without extracting effective components of rhizoma Ligustici Chuanxiong. Maxiuqin et al (China veterinary medicine journal 2020,39 (4)) have established a method for determining ligustilide in ligusticum wallichii by a quantitative nuclear magnetic resonance spectroscopy method, and do not relate to extraction, optimization and the like of main active ingredients of the ligusticum wallichii, but the method does not relate to application of an irradiation treatment technology in extraction of effective ingredients of ligusticum wallichii.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for improving the extraction efficiency of active ingredients of ligusticum wallichii by irradiation.
The purpose of the invention is realized by the following technical scheme:
a method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
firstly, drying the ligusticum wallichii, placing the dried ligusticum wallichii in a packaging bag, sealing the packaging bag, and storing the packaging bag in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode;
step three, crushing the ligusticum wallichii after irradiation;
and step four, adding an extracting agent into the crushed ligusticum wallichii, soaking in the dark, performing ultrasonic treatment, and filtering to obtain a supernatant.
Preferably, in the first step, the rhizoma Ligustici Chuanxiong is in the form of tablet, block or powder, and is dried in a dryer at 38-42 deg.C for 2-4 h.
Preferably, in the first step, the material of the packaging bag is any one of polyethylene, nylon or an aluminum-plated film composite bag.
Preferably, in the second step, the irradiation source adopts 60 Co-gamma rays or electron beams.
Preferably, in the second step, the irradiation source adopts 10 MeV electron beam energy, the thickness of the bagged powdery ligusticum wallichii is not more than 5 cm, the thickness of the flaky/blocky ligusticum wallichii is not more than 7 cm when the irradiation source is used for single-side irradiation, the thickness of the bagged powdery ligusticum wallichii is not more than 9 cm when the irradiation source is used for double-side irradiation, and the thickness of the flaky/blocky ligusticum wallichii is 13-17 cm.
Preferably, in the second step, the absorbed dose is controlled to be 1-4 kGy during the irradiation treatment.
Preferably, in the third step, the irradiated flaky/blocky ligusticum wallichii is crushed by a crusher and screened by a screen of 40-60 meshes.
Preferably, in the fourth step, the crushed ligusticum wallichii is placed into a container, the extracting agent is added, the mixture is uniformly mixed, and the mixture is soaked for 15 to 30 min in a dark place; putting the container into ultrasonic equipment, ultrasonic treating for 20-30 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Preferably, the extractant can adopt 60-80% v/v ethanol solution or 60-80% v/v methanol solution.
Preferably, the ratio of the ligusticum wallichii to the extractant is 1.
The beneficial effects of this technical scheme are as follows:
1. compared with the method for simultaneously carrying out irradiation and extraction, the method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii by irradiation needs to fully consider the packaging, the positioning and the like of a liquid mixed sample during irradiation treatment due to the addition of the liquid extractant, so that the damage to the packaging of the mixed sample is avoided; the shielding effect of liquid on rays is strong, particularly the penetration capacity of electron beams in the liquid is weak, if irradiation and extraction are carried out simultaneously, the efficiency of irradiating and processing samples is reduced, the irradiation processing is easy to be uneven, and the processing effect is influenced; in addition, after irradiation treatment, the liquid extractant can generate a large amount of free radicals which may have adverse effects on effective components in the system, and the defects can be effectively avoided by irradiating the raw materials and then extracting the raw materials. The invention carries out irradiation treatment on the raw materials, the sample is in a block shape, a sheet shape or a powder shape, and can be irradiated after being bagged, thereby being convenient and fast and having strong practicability.
2. According to the method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii by irradiation, the irradiation treatment can simultaneously and obviously improve the extraction yield of three active substances in the ligusticum wallichii, and the application range of the irradiation technology is widened. The irradiation treatment method limits the irradiation source, the product packaging thickness, the dose range, the irradiation mode, the product packaging material, the packaging mode and other related parameter ranges in the irradiation processing of the ligusticum wallichii for irradiation treatment, and the irradiation treatment must be strictly carried out according to the parameters, so that the aim of improving the yield of the three active substances through the irradiation treatment can be ensured.
3. The method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii by irradiation greatly improves the active ingredients, and the yield improvement range is about: 10.37-21.48% of ferulic acid, 4.81-13.56% of chlorogenic acid and 6.9-24.14% of n-butylphthalide.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
It will be understood that when an element is referred to as being "on," "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or intervening elements may also be present.
It should be noted that the terms of orientation such as left, right, up and down in the embodiments of the present invention are only relative concepts or are referred to the normal use state of the product, and should not be considered as limiting.
The content determination method of the effective components of the ligusticum wallichii comprises the following steps:
preparing a standard solution stock solution, and preparing an HPLC-grade standard substance: ferulic acid (CAS 1135-24-6), chlorogenic acid (CAS 327-97-9) and n-butylphthalide (CAS 6066-49-5), precisely weighing a proper amount of standard substance, dissolving in 70% (v/v) methanol, filtering with a 0.22 μm filter membrane, and storing in dark at 4 ℃ for later use, wherein the concentration range (mg/mL) of the standard substance stock solution is as follows: 0.6 to 0.8 parts of ferulic acid, 0.5 to 0.7 parts of chlorogenic acid and 0.5 to 0.8 parts of n-butylphthalide;
HPLC conditions for measuring the contents of ferulic acid, chlorogenic acid and n-butylphthalide in the ligusticum wallichii are as follows: u3000 chromatography system, C18 column (4.6 mm × 250 mm, 5 μm), mobile phase a 0.1% aqueous phosphoric acid, B acetonitrile, using a linear elution ladder: 5 to 10 percent of B for 0 to 5 min; for 5 to 15 min,10 to 30 percent of B; 30 to 40 percent of B within 15 to 20 min; 20 to 40 min,40 to 40 percent B; 40-50 min, 40-80% B; 80 to 5 percent of B is 50 to 60 min; 60-70 min, 5-5% B; detection wavelengths 230 and 280 nm; the flow rate is 1.0 mL/min, the column temperature is 30 ℃, and the sample injection amount is 10 mu L;
drawing a standard curve: taking standard solution stock solutions of three standard products, diluting the stock solutions into standard solutions with 6 concentrations in a gradient manner, performing HPLC analysis, and drawing a standard curve by taking a sample injection amount (mu g) as an abscissa and a peak area (mAU) as an ordinate, wherein the linear range (mu g) is as follows: 0.03 to 0.65 percent of ferulic acid, 0.04 to 0.92 percent of chlorogenic acid and 0.01 to 0.21 percent of n-butylphthalide;
the contents of several active ingredients in the ligusticum wallichii before and after the irradiation treatment can be calculated through a standard curve, and the effect of the irradiation treatment on the yield of the active ingredients can be obtained.
Example 1
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
drying the massive ligusticum wallichii by adopting an air-blast drying box when drying, controlling the temperature at 38 ℃, drying for 2 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of nylon, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts a 10 MeV electron beam, single-side irradiation is carried out, the thickness of the ligusticum wallichii is 5 cm, and the absorption dose is controlled to be 1 kGy;
step three, crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting 0.2 g of the crushed ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 60 percent, v/v), and soaking for 15 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Example 2
A method for improving extraction efficiency of active ingredients of Ligusticum chuanxiong Hort by irradiation comprises the following steps:
drying the flaky ligusticum wallichii by adopting an air drying box during drying, controlling the temperature at 40 ℃, drying for 3 hours, placing the dried ligusticum wallichii into a packaging bag, sealing the packaging bag, and storing the packaging bag in a dark place after the ligusticum wallichii is filled;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts 60 Co-gamma ray, during irradiation treatment, the absorbed dose is controlled to be 2.5 kGy;
step three, crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 50-mesh screen;
step four, putting 0.4 g of crushed ligusticum wallichii into a container, adding 56 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 70 percent, v/v), and soaking for 25 min in the dark; putting the container into an ultrasonic device, ultrasonically cleaning for 25 min by using an ultrasonic cleaner, cooling, supplementing the lost weight with an extracting agent, and filtering by using a 0.22 mu m filter membrane to obtain a supernatant.
Example 3
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
drying the flaky ligusticum wallichii by adopting an air drying box during drying, controlling the temperature at 42 ℃, drying for 4 hours, sealing the dried ligusticum wallichii in a packaging bag, and storing the packaging bag in a dark place after the packaging bag is filled with an aluminum-plated film composite bag;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein the irradiation source adopts 60 Co-gamma ray, during irradiation treatment, the absorbed dose is controlled to be 4 kGy;
step three, drying the irradiated ligusticum wallichii, crushing by using a crusher, and screening by using a 60-mesh screen;
step four, putting 0.6 g of the crushed ligusticum wallichii into a container, adding 120 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 80 percent, v/v), and soaking for 30 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 30 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Example 4
A method for improving extraction efficiency of active ingredients of Ligusticum chuanxiong Hort by irradiation comprises the following steps:
step one, drying powdered ligusticum wallichii by adopting an air blast drying box when drying, controlling the temperature at 38 ℃, drying for 2 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of nylon, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts 10 MeV electron beams, double-side irradiation is carried out, the thickness of the bagged powdery ligusticum wallichii is 9.0 cm, and the absorption dose is controlled to be 1 kGy;
step three, screening the ligusticum wallichii through a 40-mesh screen after irradiation;
step four, putting 0.2 g of the powdery ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 70 percent, v/v), and soaking for 15 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Example 5
A method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation comprises the following steps:
drying powdered ligusticum wallichii by adopting an air blast drying box at 38 ℃ for 1 h, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of an aluminized film composite bag, and storing the ligusticum wallichii in a dark place after the ligusticum wallichii is filled;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts a 5.0 MeV electron beam, single-side irradiation is carried out, the thickness of the bagged powdery ligusticum wallichii is 3 cm, and the absorption dose is controlled to be 1 kGy;
step three, screening the ligusticum wallichii through a 40-mesh screen after irradiation;
step four, putting 0.2 g of the powdery ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 80 percent, v/v), and soaking for 15 min in the dark; putting the container into an ultrasonic device, ultrasonically cleaning for 20 min by using an ultrasonic cleaner, cooling, complementing the lost weight with an extracting agent, and filtering by using a 0.22 mu m filter membrane to obtain a supernatant.
Example 6
A method for improving extraction efficiency of active ingredients of Ligusticum chuanxiong Hort by irradiation comprises the following steps:
firstly, drying the flaky ligusticum wallichii by adopting an air-blast drying box when drying, controlling the temperature at 40 ℃, drying for 3 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of polyethylene, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein the irradiation source adopts 60 Co-gamma ray, during irradiation treatment, the absorbed dose is controlled to2.5 kGy；
Step three, crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 50-mesh screen;
step four, putting 0.4 g of crushed ligusticum wallichii into a container, adding 56 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 60 percent, v/v), and soaking for 25 min in the dark; putting the container into an ultrasonic device, ultrasonically cleaning for 25 min by using an ultrasonic cleaner, cooling, supplementing the lost weight with an extracting agent, and filtering by using a 0.22 mu m filter membrane to obtain a supernatant.
Comparative example 1
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
drying the massive ligusticum wallichii by adopting an air drying box during drying, controlling the temperature at 38 ℃, drying for 2 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of nylon, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts 8.0 MeV electron beams, single-side irradiation is carried out, the thickness of the ligusticum wallichii is 4 cm, and the absorption dose is controlled to be 0.5 kGy;
step three, crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting 0.2 g of the crushed ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 60 percent, v/v), and soaking for 15 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Comparative example 2
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
drying the flaky ligusticum wallichii by adopting an air drying box during drying, controlling the temperature at 35 ℃, drying for 3 hours, placing the dried ligusticum wallichii into a packaging bag, sealing the packaging bag, and storing the packaging bag in a dark place after the ligusticum wallichii is filled;
step two, packaging the materialsThe rhizoma ligustici wallichii is subjected to radiation treatment in a normal-temperature low-dose mode, and a radiation source adopts 60 Co-gamma ray, during irradiation treatment, the absorbed dose is controlled to be 2.5 kGy;
step three, drying the irradiated ligusticum wallichii, crushing by using a crusher, and screening by using a 50-mesh screen;
step four, putting 0.4 g of crushed ligusticum wallichii into a container, adding 56 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 70 percent, v/v), and soaking for 25 min in the dark; putting the container into an ultrasonic device, ultrasonically cleaning for 25 min by using an ultrasonic cleaner, cooling, supplementing the lost weight with an extracting agent, and filtering by using a 0.22 mu m filter membrane to obtain a supernatant.
Comparative example 3
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
drying the flaky ligusticum wallichii by adopting an air drying box during drying, controlling the temperature at 45 ℃, drying for 3 hours, placing the dried ligusticum wallichii into a packaging bag, sealing the packaging bag, and storing the packaging bag in a dark place after the ligusticum wallichii is filled;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein the irradiation source adopts 60 Co-gamma ray, during irradiation treatment, the absorbed dose is controlled to be 2.5 kGy;
step three, drying the irradiated ligusticum wallichii, crushing by using a crusher, and screening by using a 50-mesh screen;
step four, putting 0.4 g of crushed ligusticum wallichii into a container, adding 56 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 70 percent, v/v), and soaking for 25 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 25 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Comparative example 4
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
drying powdered ligusticum wallichii by adopting an air blast drying box at 42 ℃ for 4 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of an aluminized film composite bag, and storing the ligusticum wallichii in a dark place after the ligusticum wallichii is filled;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein the irradiation source adopts 60 Controlling the absorbed dose to be 4 kGy during the irradiation treatment by using Co-gamma rays;
step three, screening the irradiated ligusticum wallichii through a 60-mesh screen;
step four, putting 0.6 g of the powdery ligusticum wallichii into a container, adding 42 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 80 percent, v/v), and soaking for 30 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 30 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Comparative example 5
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
firstly, drying the flaky ligusticum wallichii by adopting an air-blast drying box when drying, controlling the temperature at 42 ℃, drying for 4 hours, sealing the dried ligusticum wallichii in a packaging bag made of an aluminized film composite bag, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts 60 Co-gamma ray, during irradiation treatment, the absorbed dose is controlled to be 4 kGy;
step three, crushing the irradiated hemlock parsley by a crusher, and screening by a 60-mesh screen;
step four, putting 0.6 g of the crushed ligusticum wallichii into a container, adding 160 mL of an extracting agent, uniformly mixing the extracting agent with a methanol solution (the concentration of methanol is 80 percent, v/v), and soaking for 30 min in the dark; putting the container into an ultrasonic device, ultrasonically cleaning for 30 min by using an ultrasonic cleaner, cooling, complementing the lost weight with an extracting agent, and filtering by using a 0.22 mu m filter membrane to obtain a supernatant.
Comparative example 6
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
step one, taking powdery ligusticum wallichii, drying, and then adopting an air-blast drying oven for drying, controlling the temperature at 38 ℃, drying for 2 hours, and screening through a 40-mesh screen;
step two, putting 0.2 g of the powdery ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 60 percent, v/v), and soaking for 15 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Comparative example 7
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
step one, drying the massive ligusticum wallichii by adopting an air blast drying box when drying, controlling the temperature at 38 ℃, drying for 2 hours, crushing by using a crusher, and screening by using a 40-mesh screen;
step two, putting 0.2 g of the crushed ligusticum wallichii into a container, adding 16 mL of an extracting agent, and soaking the extracting agent in an ethanol solution (the ethanol concentration is 60 percent, v/v) for 15 min in a dark place; placing the container in ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, mixing, cooling, adding extractant to compensate lost weight, sealing, and performing irradiation treatment at room temperature with low dose 60 Co-gamma ray, controlling the absorbed dose to be 1 kGy;
and step three, filtering the mixture by using a filter membrane of 0.22 mu m after irradiation to obtain supernatant.
Comparative example 8
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
drying the massive ligusticum wallichii by adopting an air drying box during drying, controlling the temperature at 38 ℃, drying for 2 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of nylon, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts a 10 MeV electron beam, single-side irradiation is carried out, the thickness of the packed ligusticum wallichii is 7 cm, and the absorption dose is controlled to be 1 kGy;
step three, crushing the irradiated hemlock parsley by using a crusher, and screening by using a 40-mesh screen;
step four, putting 0.2 g of crushed ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 50%, v/v), and soaking for 15 min in a dark place; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
Comparative example 9
A method for extracting active ingredients of rhizoma Ligustici Chuanxiong comprises the following steps:
drying the massive ligusticum wallichii by adopting an air-blast drying box when drying, controlling the temperature at 38 ℃, drying for 2 hours, placing the dried ligusticum wallichii into a packaging bag for sealing, wherein the packaging bag is made of nylon, and storing the packaged ligusticum wallichii in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii in a normal-temperature low-dose mode, wherein an irradiation source adopts 10 MeV electron beams, the irradiation is carried out on a single side, the thickness of the packed ligusticum wallichii is 5 cm, and the absorption dose is controlled to be 1 kGy;
step three, crushing the irradiated ligusticum wallichii by using a crusher, and screening by using a 40-mesh screen;
step four, putting 0.2 g of the crushed ligusticum wallichii into a container, adding 16 mL of an extracting agent, uniformly mixing the extracting agent with an ethanol solution (the ethanol concentration is 85 percent, v/v), and soaking for 15 min in the dark; putting the container into ultrasonic equipment, ultrasonic cleaning with ultrasonic cleaner for 20 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
The content of the effective component of chuanxiong rhizome is measured for examples 1-6 and comparisons 1-9, and the specific data is as follows:
through the tests of examples 1-6 and comparative examples 1-9, it can be known that irradiation treatment needs to be performed on the ligusticum wallichii according to the irradiation source, the product packaging thickness, the dosage range, the irradiation mode, the product packaging material, the packaging mode and other relevant parameter ranges in irradiation processing, and the irradiation treatment needs to be strictly performed according to the parameters so as to ensure that the purpose of improving the yield of the three active substances is realized through the irradiation treatment.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modifications and equivalent variations of the above embodiment according to the technical spirit of the present invention are within the scope of the present invention.
Claims (10)
1. A method for improving the extraction efficiency of active ingredients of ligusticum wallichii by irradiation is characterized by comprising the following steps:
firstly, drying the ligusticum wallichii, placing the dried ligusticum wallichii in a packaging bag, sealing the packaging bag, and storing the packaging bag in a dark place;
step two, carrying out irradiation treatment on the packed ligusticum wallichii by adopting a normal-temperature low-dose mode;
step three, crushing the ligusticum wallichii after irradiation;
and step four, adding an extracting agent into the crushed ligusticum wallichii, soaking in the dark, performing ultrasonic treatment, and filtering to obtain a supernatant.
2. The method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii franchet by irradiation according to claim 1, which is characterized in that: in the first step, the rhizoma Ligustici Chuanxiong is in the form of tablet or powder, and is dried in a dryer at 38-42 deg.C for 2-4 h.
3. The method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii franchet by irradiation according to claim 2, which is characterized in that: in the first step, the packaging bag is made of any one of polyethylene, nylon or an aluminum-plated film composite bag.
4. The method for improving extraction efficiency of active ingredients of ligusticum wallichii franchet by irradiation according to claim 3, which is characterized in that: in the second step, the irradiation source adopts 60 Co-gamma rays or electron beams.
5. The method for improving extraction efficiency of active ingredients of ligusticum wallichii franchet by irradiation according to claim 4, which is characterized in that: in the second step, the irradiation source adopts 10 MeV electron beam energy, the thickness of the bagged powdery ligusticum wallichii is not more than 5 cm when the single-side irradiation is carried out, the thickness of the flaky/blocky ligusticum wallichii is not more than 7 cm, the thickness of the bagged powdery ligusticum wallichii is not more than 9 cm when the double-side irradiation is carried out, and the thickness of the flaky/blocky ligusticum wallichii is 13-17 cm.
6. The method for improving extraction efficiency of active ingredients of ligusticum wallichii franchet by irradiation according to claim 5, which is characterized in that: in the second step, during the irradiation treatment, the absorbed dose is controlled to be 1-4 kGy.
7. The method for improving extraction efficiency of active ingredients of ligusticum wallichii franchet by irradiation according to claim 6, which is characterized in that: in the third step, the irradiated blocky or flaky ligusticum wallichii is crushed by a crusher and screened by a screen of 40-60 meshes.
8. The method for improving extraction efficiency of active ingredients of ligusticum wallichii franchet by irradiation according to claim 7, which is characterized in that: in the fourth step, the crushed hemlock parsley is put into a container, added with an extracting agent, evenly mixed and soaked for 15 to 30 min in the dark; putting the container into ultrasonic equipment, ultrasonic treating for 20-30 min, cooling, adding extractant to make up for lost weight, and filtering with 0.22 μm filter membrane to obtain supernatant.
9. The method for improving extraction efficiency of active ingredients of ligusticum wallichii franchet by irradiation according to claim 8, wherein the method comprises the following steps: the extractant can adopt 60-80% v/v ethanol solution or 60-80% v/v methanol solution.
10. The method for improving the extraction efficiency of the active ingredients of the ligusticum wallichii franchet by irradiation according to claim 9, which is characterized in that: the ratio of the ligusticum wallichii to the extractant is 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211030884.6A CN115433079B (en) | 2022-08-26 | 2022-08-26 | Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211030884.6A CN115433079B (en) | 2022-08-26 | 2022-08-26 | Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115433079A true CN115433079A (en) | 2022-12-06 |
| CN115433079B CN115433079B (en) | 2023-12-12 |
Family
ID=84245211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211030884.6A Active CN115433079B (en) | 2022-08-26 | 2022-08-26 | Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115433079B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116999489A (en) * | 2023-08-09 | 2023-11-07 | 四川省原子能研究院 | Method for extracting tartary buckwheat flavone from tartary buckwheat bran |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1989984A (en) * | 2005-12-31 | 2007-07-04 | 天津天士力现代中药研究开发有限公司 | Chuanxiong rhizome effective ingredient, preparing method, preparation and use thereof |
| CN103755507A (en) * | 2014-02-21 | 2014-04-30 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for extracting plant total flavones through normal-temperature low-dosage irradiation |
-
2022
- 2022-08-26 CN CN202211030884.6A patent/CN115433079B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1989984A (en) * | 2005-12-31 | 2007-07-04 | 天津天士力现代中药研究开发有限公司 | Chuanxiong rhizome effective ingredient, preparing method, preparation and use thereof |
| CN103755507A (en) * | 2014-02-21 | 2014-04-30 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for extracting plant total flavones through normal-temperature low-dosage irradiation |
Non-Patent Citations (1)
| Title |
|---|
| 张晓彬 等: "辐照对川芎等中药材有效成分提取的影响", 同位素, vol. 34, no. 2, pages 111 - 119 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116999489A (en) * | 2023-08-09 | 2023-11-07 | 四川省原子能研究院 | Method for extracting tartary buckwheat flavone from tartary buckwheat bran |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115433079B (en) | 2023-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chaturvedi | Extraction of neutraceuticals from plants by microwave assisted extraction | |
| Mohan et al. | Optimization of microwave assisted extraction of andrographolide from Andrographis paniculata and its comparison with refluxation extraction method | |
| CN115433079B (en) | Method for improving extraction efficiency of active ingredients of ligusticum wallichii by irradiation | |
| CN104004106A (en) | Method for extracting effective substances in inonotus obliquus and preparation method for teabag | |
| CN108096073B (en) | Production process and application of traditional Chinese medicine oil prepared from Umbelliferae medicinal materials of Umbelliferae | |
| Mandal et al. | Microwave‐assisted extraction of total bioactive saponin fraction from Gymnema sylvestre with reference to gymnemagenin: a potential biomarker | |
| CN103655749B (en) | A kind of magnetic Extraction and enrichment method of Active Constituents in Rhubarb | |
| CN106137974B (en) | High activity inonotus obliquus powder and preparation method thereof | |
| CN101057925A (en) | Preparation technology for 'jieguqili' capsule and its quality control method | |
| Zhao et al. | Microwave-assisted Extraction of Alantolactone and Isoalantolactone from Inula helenium | |
| CN112716896A (en) | Turmeric whole extract nano-emulsion solid preparation and preparation method thereof | |
| Zhou et al. | Evaluation of microwave‐assisted extraction for aristolochic acid from Aristolochiae Fructus by chromatographic analysis coupled with nephrotoxicity studies | |
| WO2024066596A1 (en) | Rehmannia and lycium root bark decoction water extract solution, rehmannia and lycium root bark decoction water extract paste, rehmannia and lycium root bark decoction preparation and preparation method therefor, and quality control standard for rehmannia and lycium root bark decoction preparation | |
| Xiao-fei et al. | Preliminary study: biotransformation of borneol to camphor in mice, rats, and rabbits | |
| CN113559146B (en) | A kind of high-efficiency extraction method of walnut green peel polyphenols irradiated by electron beam | |
| CN103083328B (en) | The preparation method of Brassica campestris L pollen long-chain fatty acid and derivant thereof | |
| CN113759007B (en) | Quality control method of curcuma kwangsiensis | |
| CN112578029A (en) | Lung-clearing decoction preparation HPLC quality control construction method and application thereof | |
| CN105521439A (en) | Preparation method of pharmaceutical preparation for promoting blood circulation and removing stasis, diminishing inflammation and relieving pain | |
| CN115317588A (en) | Preparation method of Baoyuan decoction, baoyuan extract and Baoyuan solid preparation | |
| CN114689714B (en) | Channel warming soup control extract and preparation method thereof | |
| CN115677795A (en) | Extraction method of glucopyranoside derivative | |
| CN107158156A (en) | Agalloch eaglewood powder Chinese medicine is taken after being infused in hot water or decoction medicine materical crude slice | |
| CN108096341A (en) | Semen Ziziphi Spinosae (parched) powder Chinese medicine is taken after being infused in hot water or decoction medicine materical crude slice | |
| CN106632206A (en) | Method for improving dissolubility of proanthocyanidins of grape seed extract in press-shear assisted interaction manner |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |