2157 results about "Thin-layer chromatography" patented technology

The invention discloses preparation and application of total alkaloids extract and effective components in peganum plant seeds. The peganum plant (comprising harmel, multisectum peganum and peganum nigellastrum) seeds are heated, refluxed and extracted by ethanol, dissolved along with heat, acidulated by added 2 to 10 percent hydrochloric acid, and basified by ammonia water to separate out sediment; and the sediment is dried to obtain the total alkaloids extract mainly containing dehydrogenized peganine and peganine according to a proportion of between 0.18 to 1 and 4.30 to 1, wherein the content of the total alkaloids is more than 50 percent. The total alkaloids extract is separated by chromatography to obtain ten effective monomer components such as the dehydrogenized peganine, the peganine, and the like. Through thin layer chromatography and biological self-developing analysis, the total alkaloids extract and the effective monomer components thereof have the effect of resisting activity of acetylcholine esterase, and can be used for preparing medicament for resisting the activity of the acetylcholine esterase and medicament for treating neurodegenerative diseases.

The invention discloses a method of extracting sulforaphen. The smashed seeds of west orchids are added with two to three times as much water, the pH value is regulated to 3.8 to 4.2, ascorbic acid is added, and hydrolysis lasts seven to nine hours under the temperature of 20 to 30 DEG C; after being refrigerated and dried, the raw solution is added with fifteen to twenty five times as much propanone, supersonic extraction lasts forty to eighty minutes, and pumping filtration or double-gauze filtration follows; under the temperature of 30 to 50 DEG C, filtrate undergoes vacuum concentration in order to obtain crude sulforaphen; the crude sulforaphen is chromatographed by a silica gel column and gradiently eluted by n-hexane acetone solution, the thin-layer chromatography or HPLC tests and determines fractions containing the sulforaphen, and the crude sulforaphen undergoes vacuum concentration under the temperature of 30 to 50 DEG C; after being resolved in a small amount of acetone, the crude sulforaphen is chromatographed by a Sephadex LH-20 column, the acetone is used as eluent, the thin-layer chromatography or HPLC tests, determines and collects liquor containing the sulforaphen, and by vacuum concentration under the temperature of 30 to 50 DEG C, a sulforaphen product with eighty percent purity is produced. The method of the invention can also be used to extract the sulforaphen from the seeds of radishes, cabbages and mustards.

The invention relates to the technical field of environmental protection or chemistry analysis, which is an on-site quick detection method for organic pollutants in water; wherein on-site quick separation is carried out on various types of organic pollutants in a polluted water sample to be detected with thin layer chromatography, and on-site quick detection is carried out on the organic pollutants by using surface enhancement Raman spectroscopy technology. The method comprises the following steps of: firstly, preparing the active base of a high-density surface reinforced Raman spectrum; secondly, establishing a characteristic-peak strength-density standard curve map; thirdly, separating the organic pollutants which are stabilized on a chromatographic sheet; fourthly, obtaining the surface reinforced Raman spectrum map of the organic pollutants; and fifthly, carrying out contrast and detection. The method has the following benefits: the method has high detection and analysis speed, high sensitivity, wide detection range, low sample dosage and convenience for instrument carrying and operation; and the on-site quick qualitative analysis and semi-quantitative detection can be carried out on the organic pollutants, wherein the detective sensitivity can be less than 1 ppm.

During the extraction of resveratrol from giant knotwood, giant knotwood glycoside is hydrolyzed and enriched through organic synthesis. The extraction process includes mixing giant knotwood raw material and composite stuffing, high pressure chromatography in a high-pressure chromatographic column apparatus, gradient elution with chloroform and ethyl acetate and thin chromatographic tracking detection. The said process can reach a kilogram level yield and high product purity. The present invention may be used in extracting resveratrol and other similar product from giant knotwood material.

The invention discloses a method for extracting oligomeric proanthocyanidins, which comprises the following steps of: extracting a plant raw material containing the oligomeric proanthocyanidins with a solvent; enabling a crude extract to pass through a macroporous adsorbent resin column; eluting with water to remove protein and polysaccharide impurities; carrying out gradient elution with water and one or more selecting from alcohol, methyl alcohol and acetone as an eluant; collecting mixed solution with the volume ratio of n-butyl alcohol, acetic acid and water of 4:1:5; standing for demixing, wherein the solution at upper layer is a developing solvent; and carrying out silica gel thin-layer chromatography, wherein the elution part with the Rf value of 0.2-0.5 on a thin-layer chromatography plate is the oligomeric proanthocyanidins extract. Compared with the prior art, the invention has the advantages that the purity and the yield are both remarkably improved, the yield of the oligomeric proanthocyanidins can reach more than 80 percent, the product purity is no less than 50 percent and is basically more than 80 percent, and the method has simple and convenient process, low cost and easy industrialization.

The invention discloses a method for separating and purifying gentiamarin. A slica-gel column chromatography is adopted, wherein the particle size of column chromatography silica gel is 200 to 300 meshes, the using amount of the column chromatography silica gel is 30 times that of the weight of gentiamarin crude extract, eluent is mixed solvent of chloroform and ethanol in a volume ratio of 9:1, tracking and detection are performed by thin-layer chromatography by using a gentiamarin pure product as a contrast, the eluent is collected selectively, and the solvent is volatilized completely so as to obtain the gentiamarin pure product. By the slica-gel column chromatography, the particle size of the column chromatography silica gel, and the using amount of the eluent, the silica gel and the column chromatography silica gel are optimized, and gentiamarin can be separately eluted from a slica-gel chromatographic column in quantity according to the structural characteristics of gentiamarin, so that the extraction amount of gentiamarin is increased, and the purity of the finally obtained gentiamarin can reach 98.3 to 99.1 percent.

A method for separating a sample comprising a plurality of compounds includes loading a sample onto a planar stationary phase, said sample comprising a plurality of compounds to be separated; and, while retaining the sample on the planar stationary phase, subjecting the sample to planar electrochromatographic separation in a selected direction using a first mobile phase; and subjecting the sample to a chromatographically-based separation in a direction other than that of the direction used for planar electrochromatographic separation using a second mobile phase. Separation is optionally followed by direct detection of analytes using mass spectrometry (MS). These three dimensions of separation are orthogonal to one another, providing for improved resolution of the analytes.

The invention discloses a carbazole fluorescent probe and a preparation method and application thereof. The preparation method of the probe comprises the steps that N-ethyl carbazole-3-formaldehyde and 2,3-dimethyl benzothiazole iodide are mixed according to the molar ratio of one to one and dissolved in absolute ethyl alcohol, a mixture is heated to 150 DEG C in an oil bath, reflux reaction is conducted for 6 h, the reaction is observed to be completed by thin-layer chromatography after cooling, suction filtration and washing are conducted on the mixture, and then a red orange solid product is obtained. According to the probe, high sensitivity and selectivity are simultaneously displayed on CN-, HSO3- and pH in different systems, especially when the probe is used for detecting CN- ions, large Stocks displacement is displayed, the detection process is simple, convenient and rapid, and the detection result is accurate. Fluorescence imaging of the fluorescent probe in living cells can be obtained by combining with a laser confocal scanning microscopic technology.

The invention relates to a traditional Chinese medicament combination for treating children pharyngolaryngitis, a preparation method and a quality control method thereof; and the medicament combination consists of raw herbal materials of honeysuckle, calculus bovis, blackberry lily, tinospora root, balloonflower and radix scrophulariae, etc. According to traditional Chinese medicament conventional technology, the raw herbal materials are prepared into various preparations suitable for clinical application, including tablets, capsules, oral liquid preparations, dropping pills, granules, etc. The quality control method comprises the qualitative identification of thin layer chromatography and the content determination of high performance liquid chromatography and the like. The medicament combination is used for treating influenza, upper respiratory tract infection, and swollen sore throat, erosion of mouth and tongue, cough with profuse sputum, pharyngitis and laryngitis, tonsillitis, fever and the like caused by lung excess heat with obvious curative effect.

The invention relates to a preparation method for thiamethoxam. The preparation method comprises the following specific steps of: dissolving 3-methyl-4-nitroimidotetrahydro-1,3,5-oxadiazine and 2-chlorine-5-chloromethyl thiazole into a polar aprotic organic solvent, adding potassium iodide serving as a catalyst and potassium carbonate serving as an acid binding agent, stirring at normal temperature or in a heating way for 8 hours, and detecting whether reaction is fully completed through TLC (Thin Layer Chromatography), wherein a reaction system always keeps in yellow suspension state; and evaporating the organic solvent out, adding methylene dichloride into residues for immersion cleaning, filtering inorganic salts out, obtaining an organic phase which is a deep yellow transparent solution, evaporating the methylene dichloride to dryness, and recrystallizing the crude product by using methylbenzene to obtain maize-yellow thiamethoxam, wherein the yield is 85 percent and the purity is 98 percent. The preparation method has the advantages: the affinity substitution process is stable and quick, the tendency of a side reaction is lowered greatly, the bottleneck of the requirement on the purity of the 2-chlorine-5-chloromethyl thiazole is overcome, the problem of black color of the product is solved completely, and the product yield is greatly increased.

The invention belongs to the field of natural product isolation and relates to a purification method of alpha-mangostin. The purification method comprises the following steps: 1) crushing mangosteen shells, adding 3-10 times of a 60-80% ethanol solution to soak and extract for 2-3 times, concentrating the extract while depressurizing, adding the concentrated solution into an aqueous two-phase solvent system for extraction, collecting the organic phase, and concentrating the collected organic phase to obtain a concentrate; 2) adding water to the concentrate for dispersion, adding the dispersed concentrate to a polyamide column for adsorption, carrying out gradient elution with an ethanol solution, detecting by thin-layer chromatography, collecting the eluate, concentrating the eluate while depressurizing, and standing for crystallization; and 3) filtering out the crystals, dissolving the crystals with a mixed solution, recrystallizing, and drying to obtain alpha-mangostin. The purification method of alpha-mangostin is simple in process and easy to operate, has high product purity, and is easy to enlarge production.

The invention discloses a method for detection of an illegally added chemical in a traditional Chinese medicine preparation, which comprises the following steps: (1) carrying out thin-layer chromatography simultaneously for both sample solution containing a traditional Chinese medicine preparation to be detected and a reference substance of a chemical suspected of being illegally added; and (2) if the thin-layer chromatogram of the sample solution containing the traditional Chinese medicine preparation to be detected has spots in positions corresponding to the positions of the spots of the reference substance, performing infrared spectrum analysis for both silica gel in the positions with the spots of the traditional Chinese medicine preparation to be detected and silica gel in the positions with the spots of the reference substance, and then determining whether the traditional Chinese medicine preparation to be detected contains the chemical suspected of being illegally added. The invention can rapidly and accurately judge whether the traditional Chinese medicine preparation contains the illegally added chemical, and provides a novel method and means for detection of present adulteration of the traditional Chinese medicine preparation.

A process for extracting purified resveratrol from giant knotweed rhizome includes such steps as extracting resveratrol aglycon, concentrating by acid-catalytic hydrolyzing reaction, purifying by macroreticular resin column, eluting by water and alcohol, and examining by thin-layer chromatography.

This invention relates to a method for separating and preparing tetrahydroxy distyrene glucoside from Polygonum multiflorum. The method comprises: (1) pulverizing Polygonum multiflorum tubers, sieving to 20 mesh, extracting with water or ethanl, and concentrating the extract; (2) separating the concentrated extract with polyamide or macroporous adsorbent resin chromatographic column, eluting with ethanol, detecting by thin-layer chromatography, and collecting distyrene glucoside component; (3) vacuum-concentrating, preparing saturated solution at room temperature, cooling slowly, evaporating the solvent to precipitate crystals, vacuum-filtering, and recrystallizing to obtain white needle-like crystals of distyrene glucoside. The method has such advantages as easy operation, and high product purity.

The invention provides a peony and liquorice soup formula granule, and a preparation method and a detection method of the peony and liquorice soup formula granule. The preparation method comprises the steps of weighing peony and liquorice at a mass ratio of 1:1, adding water for decocting and extracting, merging filtrate, decompressing and condensing the filtrate to obtain a concentrated solution, drying the concentrated spray, adding water for granulating and sieving, and obtaining the peony and liquorice soup formula granule. The detection method comprises the steps of identifying the peony and liquorice soup formula granule by a thin-layer chromatography, and measuring the heavy metal content, the organo-chlorine pesticide residual amount, the fingerprint spectrum, the extract content and the paeoniflorin content of the peony and liquorice soup formula granule. The peony and liquorice soup formula granule inherits advantages of a traditional Chinese medicine single-formula granule, fully considers interaction during decocting (or other processing) of a decoction piece, and has a higher value, and the detection method allows the quality of the peony and liquorice soup formula granule to be controlled more effectively, so that the peony and liquorice soup formula granule is safer to use.

The invention relates to a pharmaceutical composition for treating chronic pharyngitis, in particular to a traditional Chinese medicinal composition for treating chronic pharyngitis, as well as a preparation method and a quality control method thereof. The pharmaceutical composition comprises figwort roots, radix asteris, radix asparagi, cortex moutan radicis, ophiopogon roots and other raw medicinal materials, and is prepared into various preparations suitable for clinical application according to traditional Chinese medicinal routine techniques, including tablets, capsules, orally taken liquid preparations, dropping pills, granules, and the like. The quality control method comprises qualitative identification for thin-layer chromatography, content determination of high performance liquid chromatography and other methods. The pharmaceutical composition has good effects of treating throat dryness, throat itch, irritable cough and other symptoms caused by chronic pharyngitis.

The invention provides a method for detecting a Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis, comprising the steps as follows: preparing a sample solution and a comparison product drug solution, adopting acetonitrile and water as mobile phases, and performing high performance liquid chromatography (HPLC) measurement, wherein the detection wavelength is 201-290nm; and detecting whether a corresponding chromatographic peak exists at a position, which has the same reservation time with the chromatograph of a comparison drug, in the chromatography of a sample. Compared with the traditional thin-layer chromatography identification method, the detection method in the invention has the advantages that the mode of processing a sample containing various drugs in a liquid phase chromatograph is changed, the mixed peak in the liquid phase chromatography except the components to be detected in the Chinese patent drug is successfully eliminated, and results are more accurate and stable.

The invention discloses a preparation method of pubescent angelica and mistletoe decoction formula granules and a quality control method thereof. The preparation method includes the steps that radix angelicae pubescentis, asarum, cassia twigs, radices sileris, ligusticum wallichii and radix angelica sinensis are extracted for obtaining volatile oil, and the volatile oil is subjected to clathration of beta-cyclodextrin; water with the weight 5-15 times the weight of total feeding amount is added to herbal residues and other nine types of medicine, and decoction and extraction are conducted twice; filtrate is subjected to vacuum decompression concentration; a concentrated solution is subjected to spray drying, spray-drying powder is obtained, and the spray-drying powder is crushed into submicron powder through an airflow pulverizer; maltodextrin and a beta-cyclodextrin clathrate compound are added to the submicron powder to be mixed uniformly, granulation is conducted through a dry method, and the pubescent angelica and mistletoe decoction formula granules are obtained. The quality control method includes the steps of infrared fingerprint spectra, thin-layer qualitative identification and HPLC content measuring. By means of the method, the advantage of drug matching can be fully played, and effective ingredients are maintained to the maximum degree; a perfect quality standard is completed, a once-measurement multi-evaluation technology of thin-layer chromatography is adopted, quality control is conducted in combination with infrared spectroscopy and chromatography, and the quality of the formula granules can be effectively controlled.

A process for extracting microcystis toxin and purifying it includes immersing microcystis in solution of acetic acid and then in methanol, removing impurities, preparing raw toxin, separating and thin-layer chromatography. Its advantages are high efficiency, low cost, high safety and purity (more than 90%), and no environmental pollution.

The invention discloses coumarin compounds. The preparation method comprises the following steps: extracting from rattan of Derris eriocarpa How by the inventor; according to the detection introduction of thin-layer chromatography, carrying out reversed-phase silica gel column chromatography, carrying out gradient elution by a petroleum ether-ethyl acetate system for further systematic separation, and recrystallizing. The antioxidation activity experiment proves that the compounds 1 have favorable antioxidation actions, the IC50 value for superoxide anion removal activity is less than that of the positive drug control ascorbic acid, the IC50 value DPPH.free radical removal activity has no great difference from the positive drug, and the compounds 1 have excellent antioxidation activity as compared with the coumarin compounds 6,7-dihydroxycoumarin, daphnetin and daphnoretin which are reported in documents. Therefore, the coumarin compounds disclosed by the invention can be used as a pharmaceutical or non-pharmaceutical antioxidant and the like.

The invention relates to the field of pharmaceutical chemistry, in particular to a synthesis method of a minodronate midbody and synthesis of minodronate. The preparation method of minodronate includes the following steps: using organic solvent to dissolve 2-aminopyridine, adding 4-acetyl chloride ethyl acetoacetate for reaction, monitoring the reaction solution by TLC(Thin-Layer Chromatography) until spots of 4-acetyl chloride ethyl acetoacetate disappear, concentrating to a dry state, dissolving concentrate in water, washing a water layer to remove impurities, extracting the water layer with the organic solvent, washing extract liquor, separating out an organic layer, conducting filtration, and concentrating the concentrate to be in a dry state, thereby obtaining A1.

The invention relates to a method for promptly detecting biogenic amine in food and belongs to the food analysis and security technical field. The method for promptly detecting the biogenic amine in food comprises the following steps: (1) extracting the biogenic amine from food samples; (2) purifying biogenic amine extracting solution; (3) derivatizing the biogenic amine extracting solution; and (4) optimizing developing solvent and analyzing thin layer chromatography. The method for promptly detecting the biogenic amine in food can be used for promptly detecting biogenic amine content in products of fish, meat, cheese, wine, vinegar and the like. Compared with the other analysis methods, the method for promptly detecting biogenic amine in food has the advantages of being free of expensive analytical instruments, low in cost, easy to operate, fast, and capable of effectively lowering monitoring cost in food production and circulation.

The invention discloses a quality detection method of a Chinese traditional patent medicine fallopia multiflora (thunb.) harald-aloe constipation relieving capsules for treating constipation. According to the quality detection method, the ginseng, the citrus aurantium, the aloe and the donkey-hide gelatin in the preparation are identified through a thin layer chromatography method while the 2,3,5,4'-tetrahydroxyl diphenylethylene-2-O-beta-D-glucoside content of the fallopia multiflora (thunb.) herald and the naringin content of the citrus aurantium in the preparation are determined by using HPLC. According to the present invention, the quality detection method has characteristics of stability, reliability, strong specificity and good reproducibility; and with the method, the quality of the fallopia multiflora (thunb.) harald-aloe constipation relieving capsules can be completely and effectively controlled, the stability of the product quality is easily achieved, the clinical medication safety and effectiveness can be ensured, and the medical and market needs can be well met.