415 results about "Solid Phase Micro Extraction" patented technology

The present invention is directed to a system for pre-treatment of a sample to be introduced in a chromatograph, and a method for performing solid-phase extraction of a component present in a sample. The system uses a syringe having a needle being provided with a porous body having a monolithic structure along at least an appropriate length of the needle and across an overall diameter of the needle. The method includes the steps of inserting the needle into the sample, passing the sample through the needle to retain an analyte within the porous body, and desorbtion of the retained analyte from the porous body.

The invention relates the device which utilizes solid adsorbent to enrich, extract, and pretreat samples on the base of nanometer fabric solid phase extractor. The device comprises 1-injector, 2-conical extraction pipe, and 3-nanometer fabric filtering medium. The head of 1 and the back opening of 2 can be connected and separated. In the 2 there are 3, and the head of 2 there is an eyelet. On the head of 2 there is 4-sampling needle which can be connected and separated with the head of 2. The invention possesses the advantages of short handling time, little dissolvent and wide application area.

The invention discloses zhuangfei strawberry essence and a preparation method thereof; the strawberry essence usually comprises faint aroma, sweet aroma, acid aroma, fruit aroma, flower aroma, and characteristic aroma, and the mass fractions of the components are 6-8 parts of faint aroma, 12-15 parts of sweet aroma, 15-25 parts of acid aroma, 40-45 parts of fruit aroma, 3-5 parts of flower aroma,and 5-8 parts of characteristic aroma. The method comprises the following steps: removing pedicles of fresh zhuangfei strawberries, washing, refrigerating and cooling the strawberries, triturating the strawberries by a triturator to obtain pasty strawberries; detecting the aroma components in ripe zhuangfei strawberry fruit by a solid-phase microextraction-gas chromatography / mass spectrum-automatic mass spectrum deconvolution identification system, and determining an optimal formula composition with reference to quantitative data of GC-MS. The zhuangfei strawberry essence obtained by the invention has good natural sense and native sense, and has better application effect in dairy and cold drink than other strawberry essence.

Disclosed is a preparation of an SPME fiber. A covalent bond method is adopted to prepare metal-organic frameworks (MOFs) as a coating for the extraction fiber. The fiber preparing method includes performing APTES amino-functionalization on a quartz fiber, namely, placing the fiber with amino on the surface into an MOF solution for reaction. An extraction device assembled by the prepared SPME coating comprises a device body, a microsyringe outer tube, a microsyringe needle, a push-pull rod and the extraction fiber with the coating, wherein the push-pull rod is arranged in the microsyringe outer tube and forms a sliding matching with the inner wall of the tube, the lower end of the push-pull rod is corroded by an aqua regia solution to obtain a corrosion end which is inserted into the extraction fiber with the coating, and a handle is arranged at the upper end of the push-pull rod. The preparation and the device have the advantages that an organic ligand of the extraction fiber coating and the MOFs is highly ordered and controllable, the extraction device has a novel structure, the coating fiber fixation is firm, and the stability and service life of the extraction fiber coating are improved.

The invention discloses a novel method for rapid detection of aflatoxin in food. The novel method studies extraction, purification and enrichment of aspertoxin in food and detects aflatoxin in food by using a combination of high performance liquid chromatography, on-line post-column photochemical derivatization and a fluorescence detector. The method employs a combination of dispersive magnetic solid-phase micro-extraction and dispersive liquid-liquid micro-extraction techniques for extraction, purification and enrichment of aspertoxin in a sample. Compared with a conventional determination method for aflatoxin, the method provided by the invention has the characteristics of a small amount of an organic solvent used in detection, short analysis time, simple operation, low detection cost, accuracy, etc.

The invention provides a method for measuring volatility phenol compound in white wine and belongs to the field of researching the white wine flavor. The method of the invention qualitatively and quantitatively analyzes the volatility phenol compound in white wine by combining the dipping solid phase micro-extraction technique (DI-SPEM) with gas chromatograph-mass spectrometer technique (GC-MS). The method of the invention can rapidly detect and accurately quantify the volatility phenol compound in the white wine by using the dipping solid phase micro-extraction technique without fussy pre-treating process. The method is rapid and simple. The accuracy of the result is promoted by using the gas chromatograph-mass spectrometer technique to detect the volatility phenol compound in the white wine. Seven phenol compounds in the measured scope have an excellent linear relationship that R2 is more than 0.99; the limit of the detection of the seven phenol compounds I is less than 7 ug / L; the relative standard deviation is less than 15%; the recovery rate is ranged between 85% and 115%. The invention provides a base for further researching the forming principle of the volatility phenol compound and has a significance to improve the quality of the white wine.

This invention relates to one method to test pyrazine compound in alcohol in liquor taste study, which applies top fix phase micro extraction and gas phase spectrum and flame thermal ion test device and uses gas phase spectrum and flare thermal ion test device cross technique in liquor with strong abnormal property of compound with good linear relation for R2>0.99 and compound test limit less than 1 mu g / L; Repeating the test relative standard bias for less than 15 percent and recycle rate larger than 80 percent.

The invention provides a simple and rapid preparation method and application of a covalent-organic framework compound solid-phase microextraction coating. According to the preparation method, the covalent-organic framework compound coating is quickly formed on quartz fiber, a device needed for the entire synthesizing process is extremely easy, and the method comprises the steps of performing amino-functionalization on the quartz fiber, impregnating surface amino-functionalized quartz fiber in a ground material precursor, repeating performing impregnating for several times, performing simple baking and cleaning the coating, so that the covalent-organic framework compound solid-phase microextraction coating can be obtained. The synthesizing method of the invention is easy to operate, requires few devices, and does not need an organic solvent, and by using the method, the covalent-organic framework compound solid-phase microextraction coating with high-temperature resistance, solvent resistance, acid and alkali resistance, high specific surface area, controllable pore size, and controllable thickness can be quickly prepared. Then the extraction coating is used to enrich environmentalpollutants polychlorinated biphenyls in water and it is detected that the coating has good enriching effects by using gas chromatography-mass spectrometry, thereby showing that the coating has good application prospect in the environment and other fields.

The invention discloses a method for quantificationally detecting phenolic compounds in solid-state fermentation products and belongs to the technical field of analysis of solid-state fermentation products. The method is mainly suitable for determination of the content of phenolic compounds in solid-state fermentation products of liquor, wherein the phenolic compounds includes yeast for preparing hard liquor, fermented grains and cellar mud. The invention particularly relates to ultrasonic extraction, headspace solid-state-phase micro-extraction and gas chromatography-mass spectrogram combined qualitative and quantitative analysis of solid-state fermentation products. The method built by the invention can be used for quickly detecting 10 kinds of volatile phenolic compounds in the solid-state fermentation products; the phenolic compounds have a favorable linear relationship R2 is more than 0.99 within a detection range; all detection limits are less than 10microgramme / L; the relative standard deviation is less than 10%; and the recovery rate is 75%-110%. The technical scheme provided by the invention is simple, convenient and quick, can be used for achieving effective monitoring of the volatile phenolic compounds in the solid-state fermentation products, and has the great significance in improving the quality of final products.

This invention relates to one method to test sulfur compound in the analysis technique, which uses top fix phase micro extraction and gas phase and color spectrum and impulse flare light tester cross technique for quantitative analysis. This invention establishes one sulfur compound test with rapid speed with limit to 0.01 mu g / L, linear relative parameter R2 less than 0.98 and with relative standard error less than 20 percent and alcohol recycle rate as 80 to 100 percent.

The invention discloses a solid phase micro-extraction device and a method for measuring volatile organic acids in tobacco leaves. The extraction device comprises a solid phase micro-extraction sample injection needle (1) and a headspace sample bottle (4), wherein a glass inner tube (5) is arranged inside the headspace sample bottle (4), a headspace bottle cover (2) is arranged at the mouth of the headspace sample bottle (4), the solid phase micro-extraction sample injection needle (1) is inserted into the headspace sample bottle (4) through the headspace bottle cover (2), and a solid phase micro-extraction fiber head (30 is mounted at the tip of the solid phase micro-extraction sample injection needle. The measurement method comprises the following steps of: weighing a tobacco leaf sample into and putting in the headspace sample bottle, adding internal standard compounds and anhydrous sodium sulfate, thoroughly mixing, sucking derivatization reagents into the glass inner tube, putting the glass inner tube into the headspace sample bottle, sealing the headspace sample bottle with the headspace bottle cover, and performing full automatic headspace solid phase micro-extraction. Compared with the prior art, the method has a simple treatment process and a high analysis speed, and is economical and practical, convenient to operate and environment-friendly.

The invention discloses a method for quickly determining ethyl carbamate (EC) in alcoholic drink, which comprises the following steps of: diluting an alcoholic drink sample to be tested into the alcoholic drink sample with final alcoholic content of 4 percent to 20 percent (v / v) by double distilled deionized water; concentrating EC in the alcoholic drink sample through a head space solid-phase micro-extraction technology without a complex preprocessing process or organic solvent; carrying out detection and quantification analysis through a gas chromatography-mass spectrometer technology; and comparing with a standard curve to calculate the content of EC in the alcoholic drink sample. The method disclosed by the invention can be used for quickly testing and determining the EC in the alcoholic drink, the detection limit can reach as low as 1.19 mug / L, the linear correlation coefficient is larger than 0.99, the recovery rate is 90.21 percent to 99.07 percent, and the relative standard deviation is less than 10 percent. The method overcomes defects of the prior determining method, and can be used for detection and quantification analysis of the EC in the alcoholic drink.

The invention relates to an electrically-driven solid phase micro-extraction method and a device thereof. An integrated porous material prepared through treating an epoxy resin as a base material, diethylenetriamine as a curing agent and polyethylene glycol as a pore forming agent and utilizing an in-situ gradual polymerization process is adopted as a solid phase micro-extraction material, the form of the solid phase micro-extraction material to prepare a solid micro-extraction column is combined with a rotation-speed-adjustable motor, a stirring effect is realized through rotation, and simultaneously the solid phase micro-extraction material which is adopted as an electrical adsorption work electrode and a platinum wire electrode which is adopted as a counter electrode are combined with a high-voltage direct current power supply to realize an electric adsorption effect in order to complete the electrically-driven solid phase micro-extraction. The electrically-driven solid phase micro-extraction method combining the electric adsorption technology with the stirring technology effectively overcomes a disadvantage that magnetic stirring cannot be used in a small-volume solution and simultaneously reduces a disadvantage that the abrasion of a solid phase micro-extraction stirring bar is easy, so the service life can be prolonged; the integrated epoxy resin based porous polymer is treated as the adsorption material, so the extraction amount and the detection sensitivity are improved. The method has the advantages of simplicity, easy operation and high flexibility.

The invention discloses a covalent organic framework compound solid phase micro-extraction fiber head and a preparation method thereof, and belongs to the technical fields of analytical chemistry andfood safety detection. A solid phase micro-extraction fiber made from a covalent organic skeleton compound is prepared, and is used to prepare the solid phase micro-extraction fiber head, and the fiber head is used for solid phase micro-extraction. The solid phase micro-extraction fiber having a covalent organic framework (COF) material coating on the surface has the characteristics of large specific surface area, porosity, large pi-pi conjugate system and large thermal stability, so the COF material has a remarkable enriching effect on aromatic compounds. The fiber head can be applied to headspace solid phase micro-extraction of volatile target substances from extraction solutions with complex matrix and direct extraction of extraction solutions with a clean matrix, and also can be applied to detection after being combined with a gas chromatograph or a gas chromatograph / mass spectrometer.

A method to detect volatile component in yellow wine belongs to technical field of yellow wine specialty analysis. The invention adopts coupled technique of roof solid phase extraction and gas phase chromatography-mass spectrum to make qualitative and semi-quantitative analysis of volatile component in yellow wine. The method can detect volatile compound in yellow wine quickly and estimate its proportion in all volatile compound initiatively. Roof solid phase extraction can complete under normal temperature without organic solvent, which avoid producing new compound during analyzing and enrich volatile component effectively. Mass spectrum detection can identify volatile component accurately to improve accuracy of the method. The invention has significance in researching micro constituent in yellow wine and improving its quality.

The invention discloses a detection method for a volatile flavor substance of an edible vegetable oil. The method comprises the following steps: (1) putting samples into a headspace bottle, preheating at 55-65 DEG C for 15-20 minutes, inserting an aged solid-phase micro-extraction head into the headspace bottle, adsorbing for 40-50 minutes, and then inserting the extraction head into a gas chromatography sampling opening, analyzing at 250-260 DEG C for 3-5 minutes, carrying out volatile flavor substance extraction and enrichment on the detected samples of the edible vegetable oil; and (2) determining chromatographic conditions, wherein the chromatographic column is 30m*0.25mm*0.25mu m of J&W DB-5MS UI capillary chromatography column; the temperature of the sampling opening is 250 DEG C; the chromatographic column is splitless; a carrier gas is high-purity helium; and the flow rate is 1.0mL / min; carrying out temperature programming; according to chromatographic condition, injecting the prepared samples into a gas chromatograph-mass spectrometer to separate and detect, and obtaining components and relative content of the volatile component of the edible vegetable oil according to the determined original chromatographic data and mass spectrometric data. The method disclosed by the invention is simple in sample pretreatment, and free of a solvent, and qualitative and quantitative analysis of the volatile flavor substance of the edible vegetable oil can be rapidly achieved.

The invention discloses red date essence and a method for preparing the same through compound enzymatic hydrolysis. The method comprises the steps of adding pectinase and cellulase to carry out compound enzymatic hydrolysis to obtain taste red date juice with dense date aroma, genuine flavor and high yield, then analyzing the active aroma ingredients of the taste red date juice by combining headspace solid-phase microextraction with gas chromatography-mass spectrometer (GC-MS) analysis; and blending the realistic and dense red date series essence with full aroma in combination with the experience accumulated over the years through the integrated application of the analysis technology and the flavor blending technology.

This invention relates to a capillary column solid phase coated with extraction phase micro extraction method and the device used with the analysis device, which comprises the following: one capillary solid phase micro extraction column with inner wall coated with solid phase, one six-way valve, extraction column heating box and transmission tube with desorption sample, micro three-way valve, micro air-extracting pump and assistant gas. The sample enters the extraction column under the assistant gas and micro air-extracting pump. After the flow and extracting of the sample, it rotates the six-way valve and immediately starts extraction column heating box to rapidly heat the capillary solid phase micro extraction column.

The invention belongs to the technical field of analysis methods for natural gas and especially relates to a carbon isotope analysis method for a series of hydrocarbon compounds in natural gas. The method comprises the following steps: step A, carrying out solid-phase micro-extraction enrichment on a series of hydrocarbon compounds in natural gas; step B, separating the hydrocarbon compounds and carrying out qualitative analysis on unknown hydrocarbon compounds; and step C, carrying out carbon isotope determination on the hydrocarbon compounds. According to the invention, solid-phase micro-extraction technology is introduced into a natural gas isotope analysis method and combined with a GC-IRMS analysis system, influence of factors like equilibrium time and equilibrium temperature on difference of adsorption capability of the hydrocarbon compounds and on carbon isotope values are analyzed, and operation conditions are optimized, so effective enrichment and carbon isotope composition analysis of the series of hydrocarbon compounds in natural gas are realized. The method provided by the invention can realize rapid and effective enrichment and carbon isotope composition analysis of the series of hydrocarbon compounds in natural gas.

The invention discloses a method for preparing a solid phase micro-extraction fiber by self-assembling a graphene coating on a metal wire serving as a carrier layer by layer, and particularly relates to a method for self-assembling graphene on the surface of a metal wire layer by layer by taking gold nano particles as connection arms. The novel method is characterized by comprising the following steps of: performing chemical silver plating on the surface of the metal wire by taking the metal wire as the carrier; and self-assembling sulfydryl functional graphene on the silver-plated metal wire layer by layer by adopting a layer-by-layer self-assembly method and taking the gold nano particles as the connection arms, and thus obtaining the novel solid phase micro-extraction fiber by self-assembling the graphene coating layer by layer. The prepared solid phase micro-extraction fiber has the characteristics of high mechanical strength, stable extraction coating, high enrichment capacity, long service life and the like, can be used for enrichment analysis of trace components in samples, such as foods, environments, medicaments, biochemical substances and the like, and has high application potential.

The present invention provides a carbon nanotube solid phase microextraction extraction head and method for preparing. The carbon nanotube solid phase microextraction extraction head includes a stainless steel fibre and a surface coating layer coating on one end of the stainless steel fibre, characterized in that the surface coating layer has a carbon nanotube. The application of the carbon nanotube can make the solid phase microextraction extraction head fire stand, have high mechanical strength, and longer service life and high enrichment times; the invention also relates three manufacturing method of the carbon nanotube solid phase microextraction extraction head, a carbon nanotube solid phase microextraction extraction head having selectively strong absorption ability to polar material or non-polar material is prepared by the selectively applied field.

The invention discloses a solid-phase micro-extraction capsule and application of the same in detection of phenol environmental estrogen in a beverage. A preparation method for the solid-phase micro-extraction capsule comprises the following steps: adding 4,4'-dipyridine and 1,2,3-benzenetricarbonic acid into a silver nitrate solution, carrying out a reaction at 150 to 170 DEG C for 2 to 4 d, and then successively carrying out cooling to room temperature, washing and drying so as to obtain a metal-organic nanotube material containing silver; and adding 0.5 to 1.5 mg of the prepared nanotube material into per 100 [mu]L of methanol, carrying out uniform dispersion, then injecting the obtained mixture into a hollow fiber film with a sealed end, then sealing the other end of the hollow fiber film and carrying out drying so as to obtain the solid-phase micro-extraction capsule. The invention also discloses a method for detecting phenol environmental estrogen in a beverage by using the solid-phase micro-extraction capsule. According to the invention, detection of multiple components of phenol environmental estrogen in the beverage is realized; and the method has the characteristics of rapidness, high efficiency, high sensitivity and the like and provides novel detection technology for quality safety monitoring of the beverage.

The invention discloses an in-tube solid-phase micro-extraction column and a preparation method thereof, and belongs to the technical field of analytic chemistry sample pretreatment. The in-tube solid-phase micro extraction column is composed of a quartz capillary tube and a graphene oxide coating layer, wherein the graphene oxide coating layer is fixed on the inner wall of the quartz capillary tube through chemical bonding. During preparation, the inner wall of the quartz capillary tube is successively washed with an acid, washed with an alkali and blown to dry by nitrogen, a toluene solution containing 3-aminopropyltriethoxysilane (APTES) is poured into the capillary tube, the capillary tube has both ends sealed and is placed in a water bath for reaction, then a graphene oxide aqueous solution activated by 1-ethyl-3-(3-dimethylaminopropyl)-carbide diimine / N-hydroxy succinimide (EDC / NHS) is poured into the capillary tube, the capillary tube has the both ends sealed and is subjected to a reaction in the water bath, the graphene oxide is allowed to be bonded to the quartz capillary tube wall, and the in-tube solid-phase micro-extraction column is obtained. The in-tube solid-phase micro-extraction column has simple and rapid preparation method, allows the graphene coating layer to have good chemical property, mechanical property and thermal stability, has high extraction capacity and long service life, and has broad application prospects in the analytic chemistry and environmental analysis fields.

The invention relates to a detection and analysis method for trans-2-nonenyl aldehyde potentiality in wort, which employs headspace solid phase micro-extraction and gas chromatography / mass spectrometry method, the method comprises the following steps: 1) sample pretreatment: placing wort in a headspace bottle for heat treatment; 2) ageing of a SPME extraction head: inserting the extraction head in a gas chromatography sample introduction for aging; 3) headspace solid phase micro-extraction: employing a solid phase extraction column to absorb a detected ingredient in upper space of the wort sample; 4) gas chromatography / mass spectrometry: editing a program, inserting the extraction head to an sample introduction port; vaporizing; introducing the ingredient from the sample introduction port to a capillary column for separating; and 5) detection: introducing the ingredient to be detected in a detector for detecting. A detection and analysis method of the present invention has the advantages of rapidity, less sample amount, accuracy, high sensitivity, no requirement of an extraction solvent and a derivative agent, no environmental pollution is generated, the environmental protection performance is good, and the detection and analysis method has no toxicity on testing staff body, and the security is high.

The invention relates to an electricity enhanced molecular imprinting solid phase micro-extraction method, characterized by: using a conductive molecular imprinting micro-extraction fiber as a working electrode, a platinum wire as an electrode and a saturated calomel electrode as a reference electrode, applying a bias voltage on the working electrode, letting a target compound be subject to electrophoresis and diffusion and migration to allow the target compound to reach the surface of the working electrode to complete the molecular imprinting identification extraction; and when extracting, providing a bias voltage to the working electrode through a electrochemical work station or potentiostat. The conductive molecular imprinting micro-extraction fiber is a metal wire with the diameter of0.5-1.0 mm, and one end of the fiber has a carbon nanotube-conductive molecular imprinting polymer composite coating with the thickness of 50-100 mu m and length of 1-2 cm. The extraction method is suitable for the extraction of ionic compounds and strong polar compounds. The conductive molecular imprinting micro-extraction fiber has simple preparation, large adsorption capacity to the target compound, high extraction efficiency, and good selectivity, can be reused more than 100 times, and has wide application prospects in the field of analytical chemistry and environmental analysis.

The invention discloses a method for determining the content of free nicotine in tobaccos and tobacco products, and the method provided by the invention comprises the following steps: carrying out solid-phase micro extraction on a tobacco powdery sample by using dimethyl polysiloxane / styrene as an extraction material; and carrying out quantitative analysis by using a gas chromatography mass spectrometer, thus obtaining the free nicotine determination result. Method evaluation data shows that the method has the advantages of accurate determination result, good reproducibility, less destructionof the balance between free nicotine and protonic nicotine and the like.

The invention relates to a method for comprehensively testing the fragrant components of crops, which belongs to the technical field of analysis and detection. The invention aims to solve a technical problem of providing a method for comprehensively testing the fragrant components of crops. Fragrant components in wheat, sorghum and maize can be comprehensively and accurately tested with the method. The method for comprehensively testing the fragrant components of crops comprises the following steps of: respectively pre-processing crop samples and capturing the fragrant components of crops with a headspace-solid phase micro-extraction method and a simultaneous distillation and extraction method, then respectively carrying out qualitative analysis through gas-phase color spectrum-mass spectrum and combining analyzed results to obtain the test results of the fragrant components of the crops. The crops refer to the wheat, the sorghum and the maize.

The invention provides an extraction head for solid phase micro-extraction, a preparation method of the extraction head and applications of the extraction head, and relates to solid phase micro-extraction. The extraction head is provided with a stainless steel substrate which is a stainless steel fiber, wherein one end of the stainless steel fiber is provided with a section of stainless steel hollow conduit and the tail end of the stainless steel fiber is provided with a zinc oxide nanorod coat. The preparation method comprises the following steps: fixing one section of stainless steel hollow conduit on the bottom end of the substrate, wherein the stainless steel hollow conduit enables one end of the coat which is close to the stainless steel hollow conduit to be always in the center of a needle tubing; preparing a zinc oxide reaction solution; adding zinc nitrate hexahydrate and hexamethylenetetramine to obtain a reaction solution; immersing the substrate in the reaction solution; reserving1-2cm stainless steel wire in a reaction bottle in order to grow the coat; sealing the reaction bottle; taking out the stainless steel wire after the reaction is finished; washing the zinc oxide nanorod coat; removing residuals from the surface and drying; and then assembling the prepared zinc oxide nanorod fiber with a 5muL micro-feeder to obtain a solid phase micro-extraction device.

The invention relates to a novel solid phase micro-extraction stainless steel fiber and a preparation method thereof, which provides a method for easily and rapidly preparing the solid phase micro-extraction stainless steel fiber with high stability and high reproducibility. The preparation method is as follows: soaking the part of cleaned stainless steel wire into acid for treatment; washing by water; ageing under the protection of nitrogen, obtaining the solid phase micro-extraction stainless steel fiber; mounting the prepared solid phase micro-extraction stainless steel fiber in a microliter syringe, obtaining a simple solid phase micro-extraction device. The method is simple in operation and low in cost. The prepared solid phase micro-extraction stainless steel fiber has excellent extraction performance on all trace amount organic pollutants. Compared with commercial solid phase micro-extraction device, the solid phase micro-extraction device has better mechanical strength and thermal stability, and has low cost and long service life. The extraction fiber has excellent application potential in fields of environmental monitoring, food hygiene and the like.