29 results about "Countercurrent chromatography" patented technology

The application relates to a high-purity melittin purification method using pH zone refining countercurrent chromatography. In order to overcome the defects of the prior art, a solvent system composed of 4-12% methyl tert-butyl ether, 42-50% n-butanol, 4-12% acetonitrile and 42-50% deionized water is used, a high-purity melittin solution is purified by using the pH zone refining countercurrent chromatography, and the finished high-purity melittin is obtained through concentration and drying. The application does not use solid fillers, does not cause loss to the sample, can almost recover all the melittin in the crude melittin, the yield is more than 90%, and the application is suitable for batch purification of high-purity melittin.

This invention belongs to the field of traditional Chinese medicine pharmaceutical technology and relates to a method for preparing aristolochic acid lactam components from Houttuynia cordata. This invention establishes a method for rapidly enriching aristolochic acid lactam components from Houttuynia cordata using high-speed countercurrent chromatography. It enriches three lactam components—aristolochic acid lactam A II, aristolochic acid lactam FI, and aristolochic acid lactam B II—from Houttuynia cordata. The enrichment process of aristolochic acid lactam components in this invention is simple, rapid, and yields high amounts, making it suitable for industrial-scale preparation. It can be used for large-scale enrichment of aristolochic acid lactam compound reference standards in traditional Chinese medicine. Furthermore, it provides essential reference standards for the safety evaluation and quality control of Houttuynia cordata, a traditional Chinese medicine for clearing heat and detoxifying.

The application discloses a preparation method of xylose, which comprises the following steps: S1, adding xylanase into a xylose mother liquor for enzyme hydrolysis and viscosity reduction; S2, adding calcium hydroxide into the enzyme hydrolysis liquor and passing in CO2 to generate nanometer calcium carbonate floccus to adsorb impurities; S3, performing cross-flow filtration on the ceramic-polyether sulfone composite membrane to improve the purity of the xylose; S4, performing multistage countercurrent chromatography separation on the calcium type strong acid cation resin, and dynamically adjusting an elution gradient through online HPLC feedback; and S5, performing three-effect evaporation concentration, then stage cooling crystallization, adding alpha type xylose crystal seeds to control the crystal form; the application utilizes enzyme hydrolysis-flocculation to cooperatively reduce the viscosity of the mother liquor to greater than or equal to 45%, and the nanometer floccus has an impurity adsorption efficiency greater than or equal to 85%; a dynamic chromatography separation factor is improved to 1.8, and the xylose recovery rate is greater than or equal to 96.2%; alpha type crystal purity greater than or equal to 99.5% is obtained through gradient crystallization, and the comprehensive energy consumption is reduced; and the enzyme hydrolysis conversion of the raffinate generates xylooligosaccharide and high fructose syrup.

This invention relates to a method for extracting and separating high-purity natural nicotine from tobacco. The invention utilizes high-speed countercurrent chromatography to prepare high-purity natural nicotine. By selecting a suitable solvent system, a system with an appropriate partition coefficient is obtained, significantly improving the separation and purification effect of nicotine. The process is simpler, more convenient to operate, results in no sample loss, is highly efficient and rapid, and allows for large-scale preparation with high purity. This invention also utilizes a eutectic solvent to extract natural nicotine from tobacco. This eutectic solvent is safe, low in toxicity, non-volatile, and reusable, making it a green and environmentally friendly solvent. The extraction method has high extraction efficiency, produces fewer impurities in the extract, and significantly reduces the amount of volatile organic solvents used, making it even more environmentally friendly.

The invention relates to the technical field of counter-current chromatographs, in particular to a high-mass-transfer separation column of a single-rotation counter-current chromatograph, which comprises a separation column bottom plate arranged on a main shaft, the power amplification plate is hung on the separation column bottom plate and connected with the ultrasonic generator, and a spiral groove is formed in the power amplification plate; the spiral pipe is embedded in the spiral groove; the spiral pipe pressing plate is arranged above the spiral pipe; the separation column top plate is arranged above the spiral pipe pressing plate; and the switching assembly is arranged on the top plate of the separation column and is used for connecting an external feeding pipe with the inlet / outlet of the spiral pipe. A plane coil pipe structure formed by winding a single continuous pipeline is adopted to replace a traditional split type combined structure, and the risk of sealing leakage of a combined surface is eliminated; interphase mass transfer online dynamic regulation and control are realized through the ultrasonic generator, so that the separation efficiency is remarkably improved; the modular design simplifies the manufacturing process, and reduces the cost and maintenance difficulty.

The invention provides a method for extracting and separating high-purity xanthohumol and isoxanthohumol by using a eutectic solvent. The invention belongs to the technical field of natural active substance extraction and purification. The method solves the technical problems of extraction, separation and purification of flavonoid effective substances in the hop residues. The method comprises the following steps: extracting residual total flavonoids of humulus lupulus by adopting a deep-eutectic solvent under the assistance of ultrasonic waves, adsorbing and enriching the total flavonoids of humulus lupulus by macroporous adsorption resin column chromatography on an extracting solution, recovering the deep-eutectic solvent, separating and purifying the enriched total flavonoids of humulus lupulus by high-speed counter-current chromatography, and purifying the total flavonoids of humulus lupulus to obtain the total flavonoids of humulus lupulus. The high-purity effective component xanthohumol and isoxanthohumol monomers are obtained. The method has the advantages that the extraction method is safe and environment-friendly, the extraction condition is mild, the yield is high, the extraction solvent can be recycled and reused for many times, a new solution is provided for utilization of hop residue waste resources, and the method has good practical application value.

The present application belongs to the technical field of depolymerization separation, and particularly relates to a method for separating polyphenolic compounds from lignin depolymerization products, the polyphenolic compounds and applications thereof. The lignin depolymerization products are mixed with an extraction liquid for extraction, the extraction products are mixed with the extraction liquid for extraction, then the obtained upper extraction liquid is cooled for crystallization, and countercurrent chromatography separation is performed to remove phenol in the depolymerization liquid. On this basis, the polyphenolic compounds are obtained through high-pressure preparation separation technology. The polyphenolic compounds obtained by the present application are functional components, and are new antioxidant active compositions. The polyphenolic compounds have high free radical scavenging rate and excellent antioxidant activity. Meanwhile, the polyphenolic compounds are lignin polyphenolic nanomicelles with fluorescence performance. The micelles can obtain strong fluorescence under a relatively short excitation wavelength. The polyphenolic compounds also have excellent anticancer activity.

The invention relates to the technical field of preparation of natural products, in particular to a high-efficiency preparation method of active ingredients of semen cassiae seeds, anthraquinone compounds are purified by adopting linear gradient countercurrent chromatography, and two gradient mobile phases are adopted: n-hexane / ethyl acetate / methanol / water (5: 5: 5: 5, v / v) and (5: 5: 8: 2, v / v); n-hexane / ethyl acetate / methanol / water (5: 5: 5.5: 4.5, v / v) and (5: 5: 7: 3, v / v) are solvent systems for internal circulation separation; n-hexane / ethanol / water (1: 1: 0.2, v / v) is used as a solvent system of an off-line two-dimensional separation mode, and the separated substances are detected and analyzed through high performance liquid chromatography to obtain nine anthraquinone compounds.

The invention provides a separation and purification method of abamectin, and belongs to the technical field of biopesticide refining. According to the invention, high-speed counter-current chromatography (HSCCC) is adopted to separate an abamectin active compound (1%-99%), and a target product is obtained. Compared with the traditional process, the method has the advantages that the high-speed counter-current chromatography is simple to operate, short in production cycle, monitorable in process and good in repeatability, the used mobile phase can be recycled, industrial wastewater generated in the process of the traditional extraction method is greatly reduced, the later wastewater treatment cost is reduced, and the process is green, environment-friendly, non-toxic and harmless. The purity of abamectin B1a in the target product is greater than or equal to 99.5%, and the purity of obtained B1b is greater than or equal to 94.5%.

The present invention belongs to the field of biomedicine, and specifically relates to an extraction method and application of an active ingredient of Shengjiang Powder that inhibits neuraminidase. The extraction method comprises the following steps: (1) preparing a crude extract of Shengjiang Powder: taking silkworm pupa, cicada shell, rhubarb, and turmeric, adding water, heating under reflux for extraction, filtering, concentrating, cooling, adding anhydrous ethanol, filtering, and concentrating to dryness to obtain a crude extract of Shengjiang Powder; (2) extracting the crude extract of Shengjiang Powder with a three-phase extraction solvent, collecting the upper phase, middle phase, and lower phase respectively, repeating the extraction 5 times, concentrating and drying to obtain extracts of each part; (3) subjecting the middle phase extract to high-speed countercurrent chromatography, using an eluent for primary separation and secondary separation according to the elution procedure, and automatically collecting the fractions; (4) concentrating and drying to obtain the active ingredient. The extracted active ingredient is applied to the preparation of a drug that inhibits neuraminidase, providing a basis for the development of such drugs.

The present invention provides a clary sage oil and a preparation method thereof. Compared with the prior art, the present invention simultaneously extracts clary sage essential oil and separates sclareol using high-speed countercurrent chromatography. The sclareol obtained by high-speed countercurrent chromatography is then added to the clary sage essential oil to produce a new clary sage oil. This new clary sage oil has a high sclareol content, is effective and targeted, and significantly improves the quality of the essential oil, with a more pronounced amber-ambergris aroma and better smoking performance. Application in cigarettes can significantly improve the smoking experience of cigarettes.

This application relates to the field of natural product chemistry, specifically disclosing a method for extracting triptolide and its application. The extraction method for triptolide includes the following steps: S1, pretreatment: After washing and drying the roots of Tripterygium wilfordii, it is subjected to ultrafine pulverization and plasma treatment to obtain Tripterygium wilfordii powder; S2, enzymatic hydrolysis: After enzymatic hydrolysis of the Tripterygium wilfordii powder, the enzyme is inactivated, centrifuged, concentrated, and dried to obtain crude triptolide; S3, purification: The crude triptolide is purified by high-speed countercurrent chromatography and vacuum dried to obtain refined triptolide. The above extraction method is simple and safe to operate, and the purity and extraction rate of the obtained triptolide are improved. The obtained triptolide can be mixed with total glucosides of paeony, glycyrrhizic acid, papain, poloxamer, xanthan gum, and propylene glycol to prepare a drug for treating rheumatoid arthritis, which has significant efficacy, high safety, and broad clinical application prospects.

This invention provides a method for the simultaneous extraction and separation of lycopene A and lycopene B from Lycium chinense root bark. Based on obtaining an effective eutectic solvent as the extractant, ultrasonic-assisted extraction is employed. Response surface methodology is used to optimize three factors significantly affecting the extraction process of lycopene A and lycopene B: extraction time, extraction temperature, and water content, thus obtaining optimal extraction conditions. Subsequently, the Lycium chinense root bark extract is passed through an ion exchange resin to remove the eutectic solvent. Finally, high-speed countercurrent chromatography (HSCLC) separation and preparative liquid chromatography (PCLC) purification are used to further obtain lycopene A and lycopene B with high purity, which are then detected and analyzed using high-performance liquid chromatography (HPLC).

The invention discloses a method for separating kinsenoside in anoectochilus formosanus by high-speed counter-current chromatography, which comprises the following steps: firstly, extracting anoectochilus formosanus with methanol, dissolving the extract with pure water after the extract is dried by distillation under reduced pressure, extracting with chloroform, drying a water layer by distillation under reduced pressure to obtain a sample, then selecting a solvent system consisting of ethyl acetate, ethanol and water (15: 1: 15), taking the following phase as a stationary phase and the upper phase as a mobile phase, the method comprises the following steps: separating and purifying a sample by adopting a tail-to-head elution mode and using high-speed counter-current chromatography, collecting a micro fraction containing kinsenoside by using a BSZ-100 type fraction collector, finally detecting by using high performance liquid chromatography, and determining the purity of the micro fraction, according to the method, the kinsenoside in the anoectochilus formosanus can be separated in one step through high-speed counter-current chromatography, the separation purity of the kinsenoside is larger than 96%, aftertreatment is simpler, and efficient and rapid preparation of the kinsenoside is achieved.

The present invention relates to a method for preparing cannabidiol by separation and purification using high-speed countercurrent chromatography, comprising: alcohol extraction and water precipitation, adsorption with a macroporous resin, and high-speed countercurrent chromatography separation. The present invention separates and obtains high-purity cannabidiol from industrial hemp flowers or leaves, while at the same time removing the psychotoxic component tetrahydrocannabinol by combining a microporous resin chromatographic column with a high-speed countercurrent chromatograph, and optimizing process parameters, and the solvent used therein being environmentally friendly, leaving no residues, having low cost and being recyclable. Therefore, the method is suitable for industrial production.

The utility model discloses a circulating device for high-speed counter-current chromatography. The circulating device comprises a plurality of control valves, a plurality of capture rings, a mobile phase storage tank, a pump, a fraction collector, a counter-current chromatography host, a detector and a chromatography workstation, the mobile phase storage tank is communicated with the pump pipeline; the pump is communicated with the counter-current chromatography host through a pipeline; the counter-current chromatography host is communicated with the detector through a pipeline; the detector is connected with the chromatographic workstation computer; circulating control valves are arranged on a pipeline for communicating the mobile phase storage tank with the pump and a pipeline for communicating the capturing ring with the fraction collector; and the capture rings are respectively communicated with the detector and the fraction collector through capture control valves through opening and closing pipelines. By arranging a plurality of capture rings connected in parallel and correspondingly arranged state switching control valves, various substances with similar solubility / partition coefficients and isomer substances contained in natural products can be circulated so as to achieve effective separation, and the purity of difficult-to-separate substances obtained after the substances are separated by the device can reach 98% or above.

Aiming at the three technical bottlenecks of low separation efficiency, high product purity and high solvent toxicity in the existing hypericin extraction and purification process, the mass transfer efficiency is improved through a steam explosion directional wall breaking technology, and the release efficiency of intracellular active ingredients is improved through multienzyme-ultrasonic coupling; multistage countercurrent chromatography separation is adopted to break through the selective limitation of traditional column chromatography on naphthdianthrone components, and the hypericin with the purity larger than or equal to 98% is finally obtained. The steam explosion technology is adopted, the dissolution rate of hypericin and other effective components is greatly increased, meanwhile, the extraction rate is increased, the yield is increased, and the cost is saved. According to the method, multienzyme-ultrasonic coupling and counter-current chromatography are combined, the problems of high energy consumption, high pollution and the like caused by strong acid (alkali) in a traditional plant extraction technology are integrally solved, oxidative deterioration caused by long-time heating of active ingredients is improved, meanwhile, the product purity is remarkably improved, and the method is suitable for industrial production. And a technical support is provided for construction of extraction production of clean, stable and high-quality natural products.

This invention discloses a highly efficient method for the enrichment and separation of isoflavones from kudzu root, belonging to the field of traditional Chinese medicine extraction and separation technology. The method includes: adsorbing and enriching kudzu root juice using HP-20 macroporous adsorption resin, optimizing the sample loading and elution conditions, and eluting with 50% ethanol to obtain a crude isoflavone extract; then separating the crude extract using high-speed countercurrent chromatography, employing a solvent system of ethyl acetate-n-butanol-water with a volume ratio of 2:1:3 to achieve efficient and simultaneous separation of four isoflavone components: puerarin, 3′-methoxypuerarin, puerarin apigenin, and daidzein. This invention features a simple process, low solvent consumption, and high separation efficiency, simultaneously obtaining multiple high-purity isoflavone monomers, making it suitable for large-scale production.

The present invention discloses a method for efficiently extracting and separating chemical components from peanut shells. The method comprises the following steps: crushing raw peanut shells, weighing the powder, adding 95% ethanol and soaking for 3 hours, heating and refluxing for extraction for 3 times, each time for 40 minutes, filtering the extract, concentrating under reduced pressure, and steaming until there is no alcohol taste. The extract is extracted twice with an equal amount of petroleum ether, discarding the petroleum ether phase, and then extracting three times with an equal amount of ethyl acetate. The extracts are combined and evaporated to dryness under reduced pressure to obtain a crude extract of raw peanut shells. The method is characterized in that the crude extract of raw peanut shells is separated using a solvent in a head-to-tail elution mode of high-speed countercurrent chromatography. The present invention can effectively separate the crude extract of raw peanut shells.

The preparation method comprises the following steps: S1, adding xylanase into xylose mother liquor for enzymolysis, viscosity reduction and degradation; s2, adding calcium hydroxide into the enzymatic hydrolysate, and introducing CO2 to generate a nano calcium carbonate flocculating constituent to adsorb impurities; s3, performing cross-flow filtration with a ceramic-polyether sulfone composite membrane to improve the purity of the xylose; s4, carrying out multi-stage counter-current chromatographic separation by adopting calcium type strongly acidic cationic resin, and dynamically adjusting the elution gradient through online HPLC feedback; s5, cooling and crystallizing by stages after triple-effect evaporation and concentration, and adding an alpha-type xylose seed crystal to regulate and control the crystal form; according to the method, the viscosity of the mother liquor is reduced by more than or equal to 45% by virtue of enzymolysis-flocculation synergy, and the impurity adsorption efficiency of nano floccules is more than 85%; the dynamic chromatographic separation factor is increased to 1.8, and the xylose recovery rate is greater than or equal to 96.2%; the purity of alpha-type crystals obtained through gradient crystallization is larger than or equal to 99.5%, and comprehensive energy consumption is reduced; and performing enzymolysis conversion on the raffinate to generate xylooligosaccharide and high fructose corn syrup.

The present invention relates to active ingredient separation and extraction technology, and specifically to a highly efficient preparation method and application of flavonoids from peanut stems and leaves. A crude peanut stem and leaf extract is subjected to gradient elution separation by high-speed countercurrent chromatography using a stationary phase, sequentially employing a first mobile phase, a second mobile phase, and a third mobile phase, to obtain daidzein and formononetin. The stationary phase comprises an upper phase of n-hexane, ethyl acetate, methanol, and water (5:4.8-5.2:1.9-2.1:7.6-8.4), the first mobile phase comprises a lower phase of n-hexane, ethyl acetate, methanol, and water (5:4.8-5.2:2.9-3.1:6.6-7.4), and the third mobile phase comprises a lower phase of n-hexane, ethyl acetate, methanol, and water (5:4.8-5.2:4.8-5.2:4.8-5.2). The present invention enables high-speed and efficient extraction of daidzein and formononetin.

The invention belongs to the field of extraction of active ingredients, and particularly relates to a preparation method for separating an anti-vascular endothelial injury active ingredient in spina gleditsiae based on high-speed counter-current chromatography, the obtained active ingredient and application. The method comprises the following steps: (1) taking spina gleditsiae, and adding ethanol for cold soaking to obtain a crude extract; (2) sequentially extracting the crude extract with a solvent to obtain a chloroform extract; and (3) carrying out high-speed counter-current chromatography on the chloroform extract to prepare compounds 1-4 at one time. According to the preparation method provided by the invention, the indole-3-formaldehyde, the (-)-syringol, the 4, 5-dihydroxybenzenol and the omega-hydroxypropylguaiacol can be obtained through large-scale, efficient and rapid purification; and the mobile phase and the stationary phase in the preparation process can be repeatedly utilized, so that the preparation cost is saved.

The invention relates to microbial polysaccharide for improving the production performance of laying hens and a preparation method thereof, and belongs to the technical field of microbial polysaccharide. The microbial polysaccharide is prepared from fermentation products of saccharomyces cerevisiae, paenibacillus polymyxa, bacillus natto and xanthomonas campestris, crude polysaccharide is extracted from fermentation liquor, then separation is conducted through high-speed counter-current chromatography, and then purification is conducted to obtain target polysaccharide. The obtained microbial polysaccharide can obviously improve the egg laying performance of laying hens.

The present invention discloses a method for screening, separating and purifying the whitening components of roses, which includes refluxing and extracting roses to obtain a crude ethanol extract; extracting the crude ethanol extract to obtain a petroleum ether extract, an ethyl acetate extract, a n-butanol extract and an aqueous layer extract; then conducting a tyrosinase inhibition activity test to determine that the ethyl acetate extract is the extract with the strongest tyrosinase inhibition activity; respectively conducting high performance liquid chromatography and microfraction activity evaluation on the ethyl acetate extract to obtain the target compounds that inhibit the activity of tyrosinase in the ethyl acetate extract; separating the ethyl acetate sample by high-speed countercurrent chromatography to obtain gallic acid and N 1 -N 5 -N 10 -tri-4-coumaroyl spermidine-rich fraction; purifying the rich fraction by semi-preparative liquid chromatography to extract gallic acid and N 1 -N 5 -N 10 -tri-4-coumaroyl spermidine. Using this method, the whitening components of roses can be accurately extracted.

The present invention relates to a preparation method and application of small molecule peptides in peanut meal, belonging to the technical field of plant small molecule peptide preparation. The preparation method of the present invention includes steps such as enzymatic hydrolysis extraction, high-speed countercurrent chromatography separation, and purification after enzymatic hydrolysis. The small molecule peptides in peanut meal prepared by the present invention have good antioxidant effects. When added to edible oil, they can significantly reduce the oxidation and rancidity during the storage of edible oil, improve the stability of edible oil, and extend the shelf life.

The invention relates to a method for preparing high-purity pinocembrin by high-speed counter-current chromatography separation, which comprises the following steps: taking propolis extract as a raw material, fully shaking a solvent system, standing for phase separation, and separately collecting an upper phase and a lower phase; the propolis extract is dissolved in an upper phase, the upper phase serves as a stationary phase, a lower phase serves as a mobile phase, high-speed counter-current chromatography is used for separation and purification, a mixed solution of the pinobufagin and the mobile phase is obtained, the mobile phase is removed, and the pinobufagin is obtained. According to the method, the high-speed counter-current chromatography technology is utilized for the first time to separate and purify the pinocembrin with the purity larger than 98% from the propolis, and the method has the advantages of no sample loss, no pollution, high efficiency, large-scale preparation, solvent recycling and the like; reagents of a solvent system adopted by the method can be recycled and reused, so that the method has a good environment-friendly function.

This invention relates to the field of separation and purification technology, and in particular to a method for extracting and separating five compounds from the pomace of red bean and blueberry. This invention develops a microwave-ultrasound synergistic enhanced extraction coupled with carbon dioxide gas-responsive in-situ eutectic solvent targeted extraction technology, combined with macroporous resin enrichment and high-speed countercurrent chromatography separation technology, achieving efficient extraction of five monomeric components: epicatechin, astragaloside, quercetin, kaempferol, and ursolic acid. This process significantly reduces time consumption, energy consumption, and environmental pollution, providing technical support for the large-scale industrial production of red bean and blueberry resources for high-value utilization.

The invention provides an anti-drug-resistant mycobacterium tuberculosis cinnamon extract I and a preparation method and application thereof, and belongs to the technical field of traditional Chinese medicine extracts.Cinnamon is used as a raw material, and the cinnamon extract I with the anti-drug-resistant mycobacterium tuberculosis effect is obtained through moving bed extraction, countercurrent chromatography separation and distillation. The cinnamon extract I disclosed by the invention has obvious anti-mycobacterium tuberculosis activity, and has a good inhibition effect on mycobacterium tuberculosis and various drug-resistant mycobacterium tuberculosis; the cinnamon extract I has no synergistic effect with common anti-tuberculosis drugs such as rifampicin, isoniazide, ethambutol, streptomycin and levofloxacin, and has no cross resistance with rifampicin, isoniazide and levofloxacin, so that the cinnamon extract I possibly has a unique antibacterial mechanism for mycobacterium tuberculosis, and a new thought and a new method can be provided for prevention and treatment of tuberculosis.

The invention provides a method for chiral separation of gossypol acetate through high-speed counter-current chromatography, and belongs to the technical field of gossypol acetate separation. According to the method, chloramphenicol alkali is used as a derivatization reagent, and gossypol acetate is synthesized into the gossypol acetate derivative by adopting pre-column derivatization. HP-beta-CD is used as a chiral selective agent and is used for a high-speed counter-current chromatography scheme for gossypol acetate derivative enantiomer separation. According to the method disclosed by the invention, the (-)-gossypol acetate and the (+)-gossypol acetate are successfully separated by limiting parameters such as a two-phase solvent system, the HP-beta-CD concentration, the pH value of an aqueous solution, the separation temperature and the like. Under the optimal conditions, the purities of the two monomer molecules both exceed 98%, and the recovery rates of the (-)-gossypol acetate and the (+)-gossypol acetate range from 80% to 90%.