29 results about "Supercritical fluid chromatography" patented technology

The invention relates to a method and a system for measuring fragrance components of essence, and relates to the technical field of essence quality identification, and the method comprises the following steps: S1, constructing a liquid chromatography-gas chromatography-supercritical fluid chromatography multi-dimensional combined analysis system, the system comprises a liquid chromatography system, a gas chromatography system and a supercritical fluid chromatography system which are connected in sequence, and S2, carrying out separation detection on essence samples from different sources or formulas by using the liquid chromatography-gas chromatography-supercritical fluid chromatography multi-dimensional combined analysis system to obtain multi-dimensional chromatographic data containing volatile and non-volatile components. According to the present invention, with the liquid chromatography-gas chromatography-supercritical fluid chromatography multi-dimensional combined analysis system, the separation problem of the aroma components with similar structures can be effectively solved, and compared with the traditional technology, the separation degree is significantly improved, and the volatile and non-volatile component information in the essence can be completely obtained.

The invention provides a method for separating EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid) through supercritical fluid chromatography, and relates to the technical field of separation and purification. The invention provides a method for separating EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid) by supercritical fluid chromatography, which comprises the following steps: by taking supercritical carbon dioxide and an organic reagent as mobile phases, and by utilizing the specific mobile phase property of supercritical CO2 after being mixed with the organic reagent (saturated aliphatic hydrocarbon) and matching with a normal-phase chromatographic column, separating the EPA from the DHA by supercritical fluid chromatography. A specific stationary phase (one or more of a silica gel surface bonded propylurea stationary phase, a silica gel surface bonded phenyl stationary phase and a silica gel surface bonded imidazolyl stationary phase) is adopted, effective separation and preparation of the EPA and the DHA in the fish oil can be achieved, the EPA and the DHA in the fish oil can be effectively separated within 50 min, the separation speed is high, the separation effect is good, and the method is suitable for industrial production. The purity of the obtained EPA and DHA is 98% or above, the purity of the EPA and the DHA is high, and the EPA and the DHA have good application prospects in the fields of medicine production and food and health care products.

The invention discloses a chromatographic peak identification method and equipment for a supercritical fluid chromatographic system and a medium, and relates to the technical field of chromatographic analysis. The chromatographic peak identification method comprises the following steps: acquiring original chromatographic data of a sample to be detected; performing noise reduction on the original chromatographic data through wavelet transform, and removing signal low-frequency components based on wavelet energy distribution to obtain a chromatogram after baseline correction; and adjusting a peak height threshold value and a slope threshold value on the chromatogram after baseline correction by using a sliding window, analyzing a signal value and a slope change trend of a detection point section by section, and determining the position of a characteristic point of a chromatographic peak. By the adoption of the method, the peak height threshold value and the slope threshold value can be dynamically adjusted, the method better fits the actual situation, the capacity of detecting weak signals and complex peak shapes is enhanced, the positions of the chromatographic peak feature points can be more finely and accurately recognized, and the precision of subsequent analysis results is effectively improved.

The invention relates to an unsaturated lipid analysis method, an unsaturated lipid analysis system and an on-line supercritical fluid derivative extraction-phase change focusing device thereof, the unsaturated lipid analysis method comprises the following steps: S1, under the action of a selective adsorbent, unsaturated lipid and a derivatization reagent are subjected to an epoxidation reaction in carbon dioxide in a supercritical state to obtain an extract liquid; the selective adsorbent is TiO2, and the derivatization reagent is m-CPBA; s2, changing the carbon dioxide in the supercritical state into a gas state by controlling the temperature and / or pressure, so as to enrich an epoxidation product of unsaturated lipid; and S3, analyzing the epoxidation product by adopting chromatography-mass spectrometry to obtain diagnosis ions of the epoxidation product, and determining the positions of double bonds in the unsaturated lipid according to the diagnosis ions. According to the method, derivation and extraction can be carried out in the same container, the extract directly analyzed by the supercritical fluid chromatography-mass spectrometry is provided, and the sample pretreatment step is simplified, so that sample degradation and artificial errors are reduced.

The invention discloses a method for preparing menadione and heptaene menadione by utilizing supercritical fluid chromatography. The method for preparing the menadione and the heptaene menadione by using the supercritical fluid chromatography comprises the following steps: dissolving a sample containing the menadione and the heptaene menadione by using a dissolving reagent to prepare a test solution; carrying out supercritical fluid chromatographic separation on the test solution to respectively prepare the menadione and the heptaene menadione; the supercritical fluid chromatographic separation conditions are as follows: a mobile phase is a mixture of supercritical CO2 and an alkane solvent; the stationary phase comprises silica gel. The provided method for preparing menadione and heptaene menadione by using supercritical fluid chromatography realizes the separation of heptaene menadione and heptaene menadione, can reduce the use of organic reagents, and has the advantages of short separation time and good separation effect.

The invention discloses a method for ultrafast specific detection of active components in tea, which comprises the following steps: obtaining extract liquor in a tea sample by supercritical extraction, and then determining the content of the active components in the tea sample by an internal standard method based on a supercritical fluid chromatography and mass spectrometry combined system, the active ingredients comprise 17 saccharides, amino acids and flavonoid substances; wherein the supercritical extraction agent is supercritical CO2 and a modifier containing formic acid, ammonium formate, water and methanol. According to the invention, 17 active components in a tea sample can be accurately detected at the same time, and the total time consumed from extraction to analysis completion of each sample is about 20 minutes; a tea sample can be directly injected and analyzed after being subjected to supercritical fluid extraction, additional purification treatment is not needed, and the analysis time and cost are remarkably saved; moreover, the method effectively reduces the interference of a sample matrix, improves the detection sensitivity, ensures the reliability of an analysis result, and can provide comprehensive and efficient information support for the research and quality control of the active components of the tea leaves.

The invention provides a method for determining vanillin by supercritical fluid chromatography, which comprises the following steps: carrying out supercritical fluid chromatography detection on a vanillin sample to obtain a detection result; a mobile phase of the mobile phase system for supercritical fluid chromatography detection comprises supercritical fluid CO2 and methanol. The method for detecting vanillin by using the supercritical chromatographic instrument is optimized and invented through combination of specific flow velocity, sample size, back pressure, modifier and the like. The method has the unique advantages of being time-saving, high in throughput, low in toxicity and eco-friendly. Compared with an existing detection method, the method has the advantages that the detection efficiency can be improved by 10 times, the sample size can be reduced by 10 times, mobile phases such as organic reagents can be reduced by 20 times, and the operation cost can be reduced by more than 50 times.

The invention provides anti-hair loss and hair growth essence and a preparation method thereof, and relates to the technical field of cosmetics. According to the anti-hair loss and hair growth essence disclosed by the invention, various natural plant extracts, amino acids, peptides and trace elements are combined and proportioned, so that the anti-hair loss and hair growth essence has the synergistic interaction functions of preventing hair loss, promoting hair growth, diminishing inflammation, inhibiting bacteria, resisting oxidation, activating blood, supplying nutrients and the like. Through introduction of green technologies such as supercritical fluid extraction-supercritical fluid chromatographic separation and the like, use and residues of organic solvents can be effectively reduced, and the enrichment degree of functional components is remarkably improved. Compared with other anti-hair-loss essence taking natural plant extracts as functional components, the essence disclosed by the invention has the advantages that the additive amount of the extracts in the essence is less, and side effects are avoided. The product has the advantages of mildness, safety, no irritation, no cleaning and the like.

The present invention provides a purification method and application of desmopressin acetate. The crude desmopressin acetate product is dissolved in an organic solvent, and the dissolved solution is filtered through an organic membrane to obtain a crude product solution; the crude product solution is separated by supercritical fluid chromatography to obtain a high-quality product solution; and the high-quality product solution is subjected to post-processing to obtain the finished desmopressin acetate product. This solution purifies desmopressin acetate with high purity in one step, greatly reducing the production cost while shortening the production cycle, and also consuming less solvent, meeting the requirements of environmental protection development.

The present invention discloses a method for ultra-rapid and specific detection of active ingredients in tea leaves. Supercritical extraction is used to obtain an extract from a tea sample, and then the content of the active ingredients in the tea sample is determined by an internal standard method based on a supercritical fluid chromatography-mass spectrometry system. The active ingredients include 17 types of sugars, amino acids, and flavonoids. The supercritical extraction agent is supercritical CO2 and a modifier containing formic acid, ammonium formate, water, and methanol. The present invention can accurately detect 17 active ingredients in tea samples simultaneously, and the total time taken from extraction to analysis of each sample is about 20 minutes. After supercritical fluid extraction, the tea sample can be directly sampled and analyzed without the need for additional purification treatment, which significantly saves analysis time and cost. Moreover, the present invention effectively reduces sample matrix interference, improves detection sensitivity, ensures the reliability of analysis results, and can provide comprehensive and efficient information support for the research and quality control of tea active ingredients.

The invention belongs to the technical field of valves, and relates to a high-pressure collecting valve suitable for being applied to a liquid chromatography system, application of the high-pressure collecting valve and a supercritical fluid chromatography system. According to the invention, high-pressure collection and automatic collection of samples in the operation process of the supercritical fluid chromatography system can be realized; the valve cavity unit adopts a scheme that equal-length branches are uniformly distributed in a star shape, so that the volume of a channel in the valve body is reduced and rectified, the dead volume of a pipeline can be greatly reduced, cross contamination among different components is reduced or even eliminated, and the sample collection rate and purity of each component are improved; the collecting valve adopts a structure completely different from a ball valve, and is provided with a pressure regulation feedback system and a sealing ring, so that the fault rate and the maintenance cost of the collecting valve can be reduced, and the service life is prolonged. The whole collecting valve adopts a modular design, so that the maintenance cost caused by hardware damage due to long-time high-pressure operation of the supercritical fluid chromatography system can be effectively reduced. And a pressure closed-loop control system is arranged, so that the collection rate and the purity of the sample can be further improved.

The present application relates to a connection device and method for supercritical fluid chromatography-mass spectrometry wherein the device comprises: a fluid introduction device for introducing a sample-containing high pressure fluid flowing out of a chromatographic column to an outlet of an ion source; the fluid outflow device is used for introducing the high-pressure fluid into the mass spectrum system and refluxing the rest of the fluid so as to maintain the pressure in the connecting device; and the pressure control device is connected with the fluid outflow device, and the pressure control device controls the pressure of the high-pressure fluid from the inlet to the outlet based on the pressure in the connecting device and the pressure of the automatic back pressure regulator ABPR so as to control the pressure in the structure to meet preset stable conditions. According to the embodiment of the invention, the fluid introduction device, the fluid outflow device and the pressure control device are included, all the parts have a synergistic effect, fluid transmission and pressure stability in a high-pressure environment are effectively guaranteed, and stable transmission of supercritical fluid is achieved by improving a flow channel structure.

This invention discloses a method for separating and preparing 4-aminoindane using a supercritical fluid chromatography (SCLC) system, comprising the following steps: dissolving an aminoindane sample; separating the aminoindane sample on a chromatographic column using a SCLC system to prepare 4-aminoindane; the mobile phase of the SCLC system is a mixture of supercritical CO2 and lower alcohols; the stationary phase of the SCLC system includes one or more of the following: silica gel surface-bonded phenyl groups, silica gel surface-bonded urea groups, or silica gel surface-bonded imidazole groups. This invention is the first to discover the use of a SCLC system for the separation and preparation of 4-aminoindane, supplementing existing high-performance liquid chromatography (HPLC); CO2 is more environmentally friendly, reducing harm to human health and the environment, and significantly reducing solvent processing costs; it can reduce the amount of chemical reagents used, reducing costs and increasing efficiency; the separation time is short, the separation effect is good, and the product purity can reach over 99%.

The invention relates to the technical field of analysis and detection, in particular to a method for detecting chiral chloropropanol ester through SFC-MS / MS. Chromatographic detection conditions are as follows: a filler type of a chromatographic column is a polysaccharide derivative chiral stationary phase, a basic skeleton is amylose, and a functional group is 3, 5-dimethyl phenyl carbamate; the mobile phase is composed of a mobile phase A, a mobile phase B and a compensation mobile phase, and the mobile phase A is carbon dioxide; the mobile phase B is a methanol solution of 0.01 wt%-0.1 wt% formic acid; the compensation mobile phase comprises methanol and / or isopropanol; the chiral chloropropanol ester comprises chiral 3-chloro-1, 2-propylene glycol palmitic acid diester, and the chiral chloropropanol ester comprises chiral 3-chloro-1, 2-propylene glycol palmitic acid diester. The invention provides a supercritical fluid chromatography-tandem mass spectrometry separation analysis method for detecting the chiral chloropropanol ester by an external standard method, does not need to add an expensive internal standard, is good in separation effect and high in precision and accuracy, and is suitable for various complex matrixes such as edible oil and the like.

The present invention provides a method for purifying digitoxin and determining its purity. Using the pure digitoxin obtained by separation and purification with supercritical fluid chromatography technology as a control, the purity of the crude digitoxin is determined by chromatography and nuclear magnetic resonance spectroscopy. The present invention uses supercritical fluid chromatography as a pretreatment means for quantitative nuclear magnetic analysis, reducing the consumption of a large amount of solvents, shortening the sample pretreatment time, avoiding interference with the measurement results such as sample degradation, and improving the efficiency and measurement accuracy of digitoxin purity determination. The present invention provides a reliable and convenient detection method for the organic purity measurement of digitoxin, and has important value in the fields of drug production, quality control and organic chemical purity analysis.

The present application is directed to methods, systems, and compositions related to and obtained from the supercritical fluid chromatography -based purification of saponins. In some embodiments, the present application is directed to methods of producing a purified saponin composition, the methods comprising applying a Quillaja saponin source composition to a supercritical fluid chromatography (SFC) stationary phase of a SFC system. In some embodiments, the present application is directed to such methods and applying an elution condition to the SFC stationary phase to produce the purified saponin composition. Also provided herein are SFC systems for practicing the methods described herein, as well as compositions and medicaments produced by the methods described herein.

The present invention belongs to the field of physical and chemical testing technology, and specifically is a method for determining phthalate compounds in water-based adhesives. The method comprises the following steps: (1) weighing a sample, dispersing it in ultrapure water, adding n-hexane, spherical carbon, and an internal standard for oscillation extraction, centrifuging, and filtering to obtain a sample solution to be tested; (2) using supercritical fluid chromatography-tandem mass spectrometry to determine and analyze the sample solution to be tested; the supercritical fluid chromatography column in the supercritical fluid chromatography-tandem mass spectrometry is Viridis HSS C18SB. The spherical carbon can effectively adsorb and purify non-target substances in the water-based adhesive. The supercritical fluid chromatography-tandem mass spectrometry analysis of phthalates in the water-based adhesive greatly shortens the chromatographic separation time, achieves good separation effect, consumes less organic solvent, and is environmentally friendly.

This invention belongs to the field of tobacco chemical composition technology, specifically relating to a method for the simultaneous analysis of multiple fat-soluble components in tobacco leaves. The method includes the following steps: drying and grinding the tobacco leaves to be tested, adding an extractant and an internal standard to obtain a sample solution; analyzing the sample using a supercritical fluid chromatography system, employing multi-wavelength detection, and using the internal standard method. This invention provides a method for the simultaneous analysis of multiple fat-soluble components in tobacco leaves, addressing the common characteristics of fat-soluble components in tobacco leaves such as large molecular weight, poor volatility, and easy oxidation and decomposition. By using supercritical fluid chromatography, it can achieve simultaneous quantitative analysis of 13 fat-soluble components in tobacco, using less solvent, lower cost, and higher detection efficiency. This provides an environmentally friendly, more efficient, and convenient high-throughput analytical method for tobacco leaf quality evaluation.

The present application is directed to methods, systems, and compositions related to and obtained from the supercritical fluid chromatography -based purification of saponins. In some embodiments, the present application is directed to methods of producing a purified saponin composition, the methods comprising applying a Quillaja saponin source composition to a supercritical fluid chromatography (SFC) stationary phase of a SFC system. In some embodiments, the present application is directed to such methods and applying an elution condition to the SFC stationary phase to produce the purified saponin composition. Also provided herein are SFC systems for practicing the methods described herein, as well as compositions and medicaments produced by the methods described herein.

The present invention discloses a method for purifying (-)-α-bisabolol from a fermentation source and preparing nano-liposomes thereof, belonging to the field of separation and purification in bio-chemical industry. In the present invention, the (-)-α-bisabolol fermentation broth is subjected to membrane separation concentration, and then based on the characteristics of (-)-α-bisabolol, a separation technology combining resin adsorption, SFE (supercritical fluid extraction) and SFC (supercritical fluid chromatography) is adopted to rapidly prepare high-purity (-)-α-bisabolol. Subsequently, the SFI (supercritical fluid injection method) technology is used to obtain nano-liposomes. The whole method avoids the extraction process, greatly reduces the use of organic solvents, reduces the risk of solvent residues and production costs. By means of the SFI technology, the deficiencies of the existing inclusion technology such as low encapsulation efficiency and cumbersome operation process are solved, and (-)-α-bisabolol nano-liposomes with uniform particle size are rapidly and simply prepared, which can improve its water solubility and permeability and broaden the application range of bisabolol.

Provided is a chiller and system that may be utilized in a supercritical fluid chromatography method, wherein a non-polar solvent may replace a portion or all of a polar solvent for the purpose of separating or extracting desired sample molecules from a combined sample / solvent stream. The system may reduce the amount of polar solvent necessary for chromatographic separation and / or extraction of desired samples. The system may incorporate a supercritical fluid chiller, a supercritical fluid pressure-equalizing vessel and a supercritical fluid cyclonic separator. The supercritical fluid chiller allows for efficient and consistent pumping of liquid-phase gases employing off-the-shelf HPLC pumps. The pressure equalizing vessel allows the use of off-the-shelf HPLC column cartridges. The system may further incorporate the use of one or more disposable cartridges containing silica gel or other suitable medium. The system may also utilize an open loop cooling circuit using fluids with a positive Joule-Thomson coefficient.

The invention provides a digitonin purification and purity determination method. A pure digitonin product obtained through separation and purification by adopting a supercritical fluid chromatography technology is used as a contrast, and the purity of the crude digitonin product is measured by utilizing chromatography and nuclear magnetic resonance spectroscopy. According to the method, the supercritical fluid chromatography is adopted as a pretreatment means for quantitative nuclear magnetic analysis, so that the consumption of a large amount of solvent is reduced, the sample pretreatment time is shortened, the interference of sample degradation and the like on a measurement result is avoided, and the purity measurement efficiency and the measurement accuracy of digitonin can be improved. The invention provides a reliable and convenient detection method for measuring the organic purity of digitonin, and has important value in the fields of medicine production, quality control and organic chemical purity analysis.

The present invention relates to a method for separating and detecting chlorfenvinphos and methyl chlorfenvinphos isomers by supercritical fluid chromatography-tandem mass spectrometry, belonging to the technical field of analytical chemistry. The method of the present invention comprises the following steps: 1) Pretreating a sample to be tested to obtain a solution to be tested; 2) Detecting the solution to be tested by supercritical fluid chromatography-tandem mass spectrometry; 3) Calculating the contents of chlorfenvinphos and methyl chlorfenvinphos isomers in the sample to be tested according to a standard working curve; in step 2), the chromatographic column used for supercritical fluid chromatography detection is packed with silica gel surface-covalently bonded with cellulose tris(3,5-dichlorophenylcarbamate), and the mobile phase is ethanol and supercritical CO2. The method of the present invention can achieve the separation and rapid quantitative analysis of cis-trans isomers of chlorfenvinphos and methyl chlorfenvinphos, with high sensitivity, high accuracy and good resolution.

The present invention discloses a high-efficiency supercritical fluid chromatography (SCF) system, relating to the technical field of chromatography. The system comprises a gas-liquid separator and a carbon dioxide filter connected by a pipeline. The gas-liquid separator is used to separate a gas-liquid mixture and convey the separated gas to the carbon dioxide filter. The carbon dioxide filter is used to filter the gas, and the filtered carbon dioxide is cooled by a refrigerator in a supercritical fluid chromatography system for reuse. The present invention can produce pure carbon dioxide in the component collection section of industrial-grade supercritical fluid chromatography, solving the problem of high carbon dioxide consumption and the inability to recycle carbon dioxide in industrial-grade supercritical fluid chromatography systems.

The invention discloses a method for purifying a fermentation source (-) alpha-bisabolol and preparing a nano-liposome, and belongs to the field of biochemical engineering separation and purification. According to the method, the (-) alpha-bisabolol fermentation liquor is subjected to membrane concentration separation, then based on the characteristics of the (-) alpha-bisabolol, the high-purity (-) alpha-bisabolol is rapidly prepared by adopting a separation technology combining resin adsorption, SFE (Supercritical Fluid Extraction) and SFC (Supercritical Fluid Chromatography), and then the high-purity (-) alpha-bisabolol is obtained by adopting an SFI (Supercritical Fluid Injection Method) technology. The nano-liposome is obtained. According to the whole method, an extraction process is avoided, the use of an organic solvent is greatly reduced, and the risk of solvent residue and the production cost are reduced. By means of the SFI technology, the defects that an existing inclusion technology is low in encapsulation efficiency, tedious in operation process and the like are overcome, the (-) alpha-bisabolol nano-liposome with the uniform particle size can be rapidly, simply and conveniently prepared, the water solubility and permeability of the (-) alpha-bisabolol nano-liposome can be improved, and the application range of bisabolol can be widened.

The invention relates to an ultra-efficient supercritical fluid chromatography stationary phase as well as a preparation method and application thereof. The stationary phase is ordered mesoporous silica gel microspheres or ordered mesoporous inorganic / organic hybrid silica gel microspheres. The ultra-efficient supercritical fluid chromatography stationary phase is a material which is uniform in pore size distribution, ordered in pore structure and controllable in morphology and is obtained by a soft template method. The separation material prepared by the invention can obtain ultrahigh column efficiency in supercritical chromatography, meanwhile, due to the property of large specific surface area, the retention of weak polar compounds is enhanced, and the problems of weak retention and poor separation effect of different lipid-soluble samples in supercritical chromatography are solved. The preparation method is simple in process and mild in reaction condition, has good preparation reproducibility and stability, and is easy to popularize and apply.