213 results about "Accelerated solvent extraction" patented technology

The invention belongs to the technical field of physicochemical testing of residual pesticide in tobacco and a tobacco product and in particular to a method for mensurating the residual amounts of six classes of dinitraniline pesticides, The method is to extract residual pesticides in an accelerated solvent extraction instrument (ASE), and use a gas chromatograph (matched with electron capture detector (ECD) to directly mensurate the residual amounts of six classes of the dinitraniline pesticides in the tobacco and the tobacco product, namely, butralin, flumetralin, isopropalin, pendimethalin, benfluralin and trifluralin. The method overcomes the disadvantages of a sample treatment method in the prior art and optimizes a sample pretreatment method and the instrument detecting conditions aiming at a tobacco sample. Compared with the prior art, the method has the advantages of simple pretreatment process, reduction of the interference of pigment and other impurities in the tobacco, high automation degree of the whole operation, accurate operation, high sensitivity and good repeatability.

The invention discloses a method for detecting the content of a triocresyl phosphate fire retardant of a rubber part of an electrical or electronic product. The method comprises the following steps of: (1) sample preparation; (2) extraction of the triocresyl phosphate fire retardant: adding heavy metal powder into the sample, uniformly mixing and performing accelerated solvent extraction so as to obtain extract; (3) extract purification: uniformly mixing the extract and an interior label, transferring to a small solid phase extraction column, eluting by using a mixed solvent, collecting and concentrating eluent so as to obtain the purified extract; and (4) measurment of the triocresyl phosphate fire retardant: measuring the purified extract and the triocresyl phosphate mixed standard solution containing the interior label by using a gas chromatography-mass spectrometer, and performing data processing and quantitative analysis to obtain the content of the triocresyl phosphate fire retardant. By the method, interference impurities in the rubber can be eliminated effectively, triocresyl phosphate can be extracted fully, the purification degree is high, the detection sensitivity is high and the sample measurement cost is low.

The invention discloses a passive sampler for polycyclic aromatic hydrocarbon in indoor air and a sampling testing method thereof and belongs to the fields of sampling and determining of the polycyclic aromatic hydrocarbon. The sampler comprises a sampling bottle and a sampling support, the sampling bottle is filled with granular CarbotrapB or XAD-4 resin which serves as an adsorbent, and the sampling support is a double-layer metal support. Sampling testing steps comprise washing adsorbent; inversely placing the sampling bottle filled with the adsorbent at the position of a circular hole of the upper layer of the sampling support for sampling; extracting the polycyclic aromatic hydrocarbon in the adsorbent; determining quality Mg, i of 15 kinds of PAHs obtained by sampling of the passive sampler through gas-mass chromatography; determining sample rate through fitted line slope fitted by Veq-t; and calculating mean concentration Cg, i of the polycyclic aromatic hydrocarbon in the indoor air. The passive sampler is simple in manufacture and assembly and low in cost, only uses accelerated solvent extraction to extract the polycyclic aromatic hydrocarbon in the adsorbent, greatly reduces use of organic solvent, shortens analysis time and is applicable to sampling of the polycyclic aromatic hydrocarbon in the indoor air.

The invention relates to a method for simultaneously extracting and purifying a plurality of types of chlorinated polycyclic aromatic hydrocarbons in soil. The method comprises the following steps of: pre-treating a soil sample, namely putting a pre-frozen soil sample into a freezing dryer, and freeze-drying to remove moisture; grinding the freeze-dried soil sample and sieving with a 200-mesh sieve to prepare soil for later use; accelerating solvent extraction; extracting a target matter by utilizing a water solution under high temperature and high pressure to obtain an extracting solution; after diluting the extracting solution for 5 times, carrying out concentration and purification by adopting an Oasis HLB solid-phase extraction column; carrying out rotary evaporation and nitrogen blowing concentration on the concentrated and purified extracting solution; after replacing a solvent, making the volume constant; then transferring the extracting solution into a small bottle for detecting; and detecting the sample in the small bottle by utilizing a gas chromatographic-mass spectrometry. By combining a plurality of types of technologies including subcritical water solution-solvent extraction acceleration, solid-phase extraction, concentration and purification, and gas chromatographic-mass spectrometry detection and the like, simultaneous extraction, purification and determination of eight types of the chlorinated polycyclic aromatic hydrocarbons in the soil can be realized.

The invention discloses electronic cigarette tobacco liquid with functions of relieving cough and moistening lung. The electronic cigarette tobacco liquid is prepared from the following components in parts by weight: 1-10 parts of tobacco extract, 30-45 parts of propanediol, 30-45 parts of glycerol, 10-15 parts of food extract capable of relieving cough and moistening lung and 0.5-1 part of nicotine. The food extract capable of relieving cough and moistening lung is an extract of one or more of water chestnuts, kumquats, snow pears, loquats, lotus roots, sugarcanes and lilies and is extracted by adopting an ethnal water solution accelerated solvent with the concentration of 10%. The electronic cigarette tobacco liquid with the functions of relieving cough and moistening lung has no injury of second hand smoking and does not influence the health of people around; meanwhile, the electronic cigarette tobacco liquid contains the food extract capable of relieving cough and moistening lung, is safe and has no toxic side effect, and has the effects of moistening lung and reducing phlegm; the electronic cigarette tobacco liquid can be used for effectively preventing and relieving discomforted symptoms including cough, throat itch and the like, caused by smoking.

The invention provides a determination method for arsanilic acid, nitarsone and roxarsone in an animal foodstuff. The invention is characterized in that the determination method comprises the following steps: weighing A g of a to-be-determined sample, placing the sample in a mortar, adding 3A g of Florisil, carrying out full mixing with stirring, using an accelerated solvent extraction instrument for extraction, wherein an aqueous methanol solution with a volume ratio of methanol to water of 3: 7 is used as an extraction solvent, and allowing a constant volume of 5A ml to be obtained through addition of water after completion of extraction; and carrying out filtering with a filter membrane and carrying out determination by using liquid chromatography-atomic fluorescence spectroscopy; wherein A is an integer not equal to zero. Compared with the prior art, the invention has the following advantages: the method for simultaneous determination of residual quantities of arsanilic acid, nitarsone and roxarsone in animal derived food by using accelerated solvent extraction-liquid chromatography-atomic fluorescence spectroscopy is researched and established in embodiments in the invention; the proportion of the extraction solvent, extraction temperature, extraction time and extraction frequency of accelerated solvent extraction technology are optimized, and the advantages of a small usage amount of the extraction solvent, rapidness, small influence on a matrix, high extraction efficiency and good selectivity are obtained.

The invention discloses a method for extracting linarin from wild chrysanthemum flower, which comprises the following steps: 1. pulverizing wild chrysanthemum flower, passing through a 50-mesh screen, and mixing with diatomite; 2. extracting linarin by ASE (accelerated solvent extraction), and collecting the extracting solution, wherein the extraction solvent adopted by the ASE is methanol; and 3. carrying out centrifugal separation on the extracting solution to obtain the linarin-containing supernate. The method has the advantages of high extraction speed and high precision.

The invention belongs to the technical field of environmental protection and pollution control, and in particular relates to a device for remediation of organic contaminated soil by using supercritical CO2 fluid and a remediation method. The device of the invention is composed of a CO2 storage tank, a pressure pump, an inlet valve, a pressure monitoring device, a soil pretreatment device, a stirring extraction vessel, a temperature control device, a pressure reducing valve, a gas-liquid separator, an organic pollutants storage tank and an organic pollutants filtering device. The method of the invention has the characteristics such as short extraction time, less solvent consumption, easy operation, high extraction efficiency, no pollution, and highly selective extraction realized through changing extraction conditions. Compared with traditional extraction techniques such as Soxhlet extraction, ultrasonic extraction, and accelerated solvent extraction, the method of the invention has the advantages such as short extraction time, no need of pre-concentration and purification, and no secondary pollution generated.

The related extraction device applied with gas phase chromatogram on-line comprises: a small extraction pond, a heating unit, a ten-way valve, a six-way valve, a dosing tube, an assist carrier gas, a stead valve, a pressure sensor, a high-pressure pump for solvent, and a capillary transmission pipe. Compared with prior art, this invention improves sample utility up to 50-100 times with less solvent and high repeating precision, and has wide application.

The invention discloses a test method for the residual phthalate ester, including the steps that after a solid sample is decomposed into blocks which are immersed in the dummy body fluid, the transferring amount of the phthalate ester in the solid sample under the condition with the dummy body fluid can be obtained through the auxiliary lixiviation by water bath ultrasound, the purification and the enrichment of solid extraction columellas filled with multi-walled carbon nano-tubes, and the measurement by a gas mass spectroscopy; and meanwhile, after the solid sample is decomposed into blocks, the total content of the phthalate ester in the solid sample can be obtained through the extraction by an accelerating solvent extraction method, the purification and the enrichment of small solid extraction columns filled with multi-walled carbon nano-tubes, and the measurement by a gas mass spectroscopy. The invention has the advantages of less dosage of organic solvent, rapid extraction speed, less impurity interference, high sample recovery ratio, and the like. In addition, prefilled small solid extraction columns are made from the multi-walled carbon nano-tubes, thereby the enrichment effect of the phthalate ester in the dummy body fluid extract of samples to be tested can be greatly improved, and a phthalate ester hazard evaluation system can be better perfected according to the difference of the total residual quantity and the dissolved quantityof phthalate ester in the solid sample.

The invention provides a method for testing water deposits or estrogen coalitions in soil. Water deposits or four estrogen coalitions, namely E1-3S, E2-3S, E1-3G and E2-3G in soil are tested by a technology combining ASE (Accelerating Solvent Extraction), SPE (Solid Phase Extraction) and LC/ MS/ MS (Liquid Chromatography/ Mass Spectrum/ Mass Spectrum), and the estrogen coalitions in the deposits are extracted by using an extractant in which the ratio of acetonitrile to water (v/v) is 9:1 as an accelerating solvent. After extract is primarily purified by a NH2 column, an HLB column is used for further purification. The extract is primarily purified by the NH2 column, substances with strong nonpolarity can be removed, the influence of matrix interference on the later enrichment of the HLB column is weakened, and the purifying effect and the recovery rate are improved. The recovery rates of the four estrogen coalitions E1-3S, E2-3S, E1-3G and E2-3G with the method are all between 83% and 108%, the testing limit is lower than 0.04ng/g, and the detection requirement on the trace estrogen coalitions in the deposits or the soil samples is met.

The invention relates to multifunctional heating pressurized extraction-trapping-chromatographic separation on-line combined equipment. The multifunctional heating pressurized extraction-trapping-chromatographic separation on-line combined equipment comprises four chromatographic pumps, three three-way mixers, two six-way switching valves, a heating pressurized extraction unit, a trapping column, a chromatographic column, a detector and the like. Through combined use of an on-line trapping-desorption-switching device and an extraction-chromatographic separation device, switching of the two high-pressure six-way switching valves and pressure adjustment of a back pressure regulator are controlled, the two extraction modes, including supercritical fluid extraction and accelerated solvent extraction, and the two chromatographic techniques, including supercritical fluid chromatography and high performance liquid chromatography, can be freely combined for use, functional diversity of the equipment is improved, and the multifunctional heating pressurized extraction-trapping-chromatographic separation on-line combined equipment can be effectively used for on-line extraction, trapping, desorption, separation and detection of trace objects in such complicated solid or semi-solid samples as environments, food, medicines and biology.

The invention provides a method for detecting a plurality of residual pesticides in tobacco simultaneously. The method is characterized by carrying out sample pretreatment by an ASE (accelerated solvent extraction) device so that extraction and purification are realized through one step, wherein a florisil and graphitized carbon black (GCB) mixture is added to an accelerated solvent extraction tank at the bottom of which a filter membrane is arranged; next, a mixed sample, which is a mixture of powdered tobacco and kieselguhr, is added to the accelerated solvent extraction tank; in succession, an interior label is added and the unoccupied space above the extraction tank is fully filled with the kieselguhr; after extraction is finished, the extracts are mixed evenly and filtered through a 0.22-micron organic phase filter membrane; finally, liquid chromatography-tandem mass spectrum (LC-MS/MS) detection is carried out. The method provided by the invention is capable of completing the extraction and purification of the sample through one step so that the pretreatment process is greatly simplified; the detection method is high in automation degree, simple to operate, high in sensitivity and accuracy, and good in repeatability; the method is capable of detecting as many as 92 residual pesticides in the tobacco simultaneously, and meets the requirements of a multiple-residual pesticide analysis method.

The invention discloses a method for detecting polycyclic aromatic hydrocarbon in ambient air. The method includes steps of 1), continuously collecting ambient air samples in sampling points by the aid of ambient air sampling instruments; 2), extracting polycyclic aromatic hydrocarbon in the samples by the aid of accelerated solvent extraction processes; 3), purifying obtained extract liquid by the aid of column chromatography processes after extraction is completely carried out; 4), concentrating fraction collected after column chromatography is carried out; 5), carrying out detection by the aid of gas chromatography-triple quadrupole rods tandem mass spectrometry; 6), qualitatively and quantitatively analyzing the samples and calculating the content of the polycyclic aromatic hydrocarbon in the ambient air. The method has the advantages that the multiple samples can be simultaneously collected, impurity removal and purification can be carried out on the samples, accordingly, interference of various matrixes on the actual samples can be eliminated, and the polycyclic aromatic hydrocarbon in the ambient air can be detected by the aid of gas chromatography-triple quadrupole rods tandem mass spectrometry processes; the method is good in sensitivity and high in selectivity, and quick and effective detection results can be obtained.

The invention discloses a method for the combined use of accelerated solvent extraction and high speed countercurrent chromatogram and a device thereof. An accelerated solvent extraction device extracts a material so as to obtain an extraction liquid which is collected by a liquid storage bottle. The extraction liquid is pumped by a peristaltic pump into a dosing ring. Stationary phase in the liquid storage bottle is pumped by a plunger pump into a high speed countercurrent chromatography. The high speed countercurrent chromatography is started, and simultaneously the plunger pump is used forpumping flowing phase in the liquid storage bottle into the high speed countercurrent chromatography for purpose of solvent system balance. Sample solution in the dosing ring is pumped into the high speed countercurrent chromatography. A preparing-type high speed countercurrent chromatogram is used for purification and preparation so as to obtain a target component, or an analysis-type high speedcountercurrent chromatogram is used for analyzing the target component in a natural product extract liquid. The above steps are integrated with the accelerated solvent extraction and the high speed countercurrent chromatogram by utilizing a switch valve, thereby realizing the online extraction, separation, purification and preparation of the natural product effective component and having the advantages of fastness, high efficiency and high automation. The method and the device have a wide application prospect in the fields such as food, medicine, biology and the like.

The invention discloses a method for treating a pesticide residue sample in a Chinese medicinal material before measurement. The method comprises the following steps of: accurately weighing the treated Chinese medicinal material sample and uniformly mixing with diatomite; adding a cellulose filter membrane at the bottom of an extraction tank; charging the mixed sample from the bottom for accelerated solvent extraction; statically extracting for 5 minutes under the conditions that the temperature is 100 DEG C, the volume ratio of the acetone to the normal hexane is 1:9 (v/v) and the pressure is 1,500psi, and extracting for 2 circulations; collecting the extract, concentrating to nearly dry, and blowing nitrogen to dry; adding the mixed solution of the acetone and normal hexane or an acetonitrile organic solvent for dissolving; and performing purification treatment to obtain supernatant, and fixing the volume for later measurement. Due to the adoption of the technology of accelerated solvent extraction, the method has the advantages of short detection flow, convenient operation, recovery rate of 70 to 110 percent, and high sensitivity, can detect 60 pesticide residues in the medicinal material simultaneously, and has good application prospects.

The invention discloses a method for simultaneously determining four components in semen ziziphi spinosae by adopting an accelerated solvent extraction-charged aerosol detector and aims at providing a method for simultaneously determining the four components in the semen ziziphi spinosae by adopting the accelerated solvent extraction-charged aerosol detector which is efficient, accurate and good in reproducibility. According to the technical main points, the method comprises the steps of (1) preparing a reference substance stock solution; (2) preparing a test sample solution; and (3) injecting a reference substance solution and the test sample solution into chromatograph for detection separately, wherein a chromatographic column is Thermo Synronis C18, a mobile phase is acetonitrile-water, the gradient elution program is 10-60% of acetonitrile and 90-40% of water for 0-8min, 60-80% of acetonitrile and 40-20% of water for 8-10, 80-100% of acetonitrile and 20-0% of water or 10-13min, and 100% of acetonitrile for 13-16min, the flow rate is 0.5mL.min<-1>, the column temperature is 40 DEG C, the atomization temperature is 35 DEG C and the sample size is 1muL. The method belongs to the technical field of chemical detection.

The invention discloses a method for detecting the polybrominated diphenyl ether content in a sludge composting sample by using an accelerated solvent extraction online purification method. The methodcomprises: treating a sludge composting sample; filling the extraction pool of an accelerated solvent extraction instrument; setting extraction conditions; and after concentrating the extraction liquid, detecting by using a gas chromatograph-mass spectrometer. According to the present invention, according to the characteristics of the sludge composting sample and the characteristics of the targetsubstance polybrominated diphenyl ether, the graphitized carbon black as the key filling material, magnesium silicate, an acidic silica gel and other materials are mixed, and the extraction pool of the accelerated solvent extraction instrument is filled with the obtained mixture, such that the accelerated solvent extraction instrument can extract 14 kinds of polybrominated diphenyl ethers in thesludge composting sample, and can further perform online purification on the sample, wherein the concentrated extraction liquid can be directly subjected to analysis detection by the gas chromatograph-mass spectrometer (NCI mode); and the method has advantages of high recovery rate, greatly-shortened sample pretreatment time, reduced organic solvent consumption and sample treatment cost reducing.

The invention discloses a method for synchronously extracting and purifying various chlorinated polycyclic aromatic hydrocarbons in soil, which belongs to the field of detection of the chlorinated polycyclic aromatic hydrocarbons. The method comprises the following steps: firstly removing moisture in a soil sample by virtue of a freezing dryer, grinding the soil sample, and filtering the ground soil sample by virtue of a 200-mesh sieve for later use; and extracting a target matter in the soil sample by utilizing an acceleration solvent extractor, purifying the target matter in a gel permeation chromatography, finally concentrating the target matter and sizing the target matter. According to the method, a preprocessing method of the chlorinated polycyclic aromatic hydrocarbons in the soil is established, less solvent is used in the entire process, the automation degree is high, less time is used, the safety is high, fewer steps are used, and various chlorinated polycyclic aromatic hydrocarbons in the soil can be accurately, qualitatively and quantitatively determined. The chlorinated polycyclic aromatic hydrocarbons in the soil are quantitatively detected by utilizing the gas phase chromatography-mass spectrometry, the detection limit is low (when S/N is equal to 3, the detection limit is 2.6 to 25pg/g), the precision is high (RSD=6.30 to 12.0 percent), the blank mark recovery rate is 64.1 to 109.2 percent, the synchronous analysis and detection of various trace chlorinated polycyclic aromatic hydrocarbons in the complicated environment medium such as the soil can be realized, sensitivity and accuracy can be realized, and the weaknesses of the prior art can be overcome.

The invention discloses a preparation method of algal oil DHA. The preparation method comprises following steps: 1, selected microalgae is subjected to algae seed culturing and heterotrophic fermenting so as to obtain a microalgae raw material; 2, the microalgae raw material is subjected to drying treatment so as to obtain microalgae powder; 3, the microalgae powder is subjected to microalgae wallbreaking pre-treatment so as to obtain dried microalgae powder; 4, algal oil is extracted, wherein the dried microalgae powder is taken as a raw material, an ethanol solution with a mass concentration of 60 to 100% is taken as an extractant, an accelerated solvent extraction instrument is adopted for extraction, an obtained extract is introduced into a vacuum rotatory evaporator for organic solvent evaporation, and a residue obtained through evaporation is the algal oil; 5, urea coating enrichment purifying is carried out; and 6, filtering condensation is carried out so as to obtain algal oilDHA finished products. The product purity of the preparation method is high, defects in preparation of DHA from fish oil and microalgae are avoided, and the finished product can be taken as a raw material in the fields of food, health care product, food additive, and high grade chemical product.

The invention discloses a method for synchronous determination of the content of triazole chiral pesticide enantiomers. According to the method, the technology of accelerated solvent extraction is used to treat a soil sample, an online polarimetric optical detector is used to determine the eluting sequence of the enantiomers, and the methods of reverse phase liquid chromatography with a chiral stationary phase and triple quadruple tandem mass spectrometry are utilized for synchronous determination of enantiomers of nine triazole chiral pesticides, namely, hexaconazole, flutriafol, diniconazole, cyproconazole, tetraconazole, epoxiconazole, myclobutanil, fenbuconazole and triadimefon; the detection limit of the method is as low as 0.5 to 1.0 mu g/kg.

The invention discloses a high-throughput analysis method for identifying hazardous waste substances in solid wastes. The method comprises the following steps: freeze-drying, grinding and sieving: freeze-drying a solid waste sample by a freeze-dryer, grinding the freeze-dried solid waste sample by a mortar and sieving by a sieve; accelerated solvent extraction: extracting organic matters in the solid waste sample by an accelerated solvent extractor; concentration and constant volume realization: concentrating extracting solution and performing constant volume on the extracting solution, filtering the extracting solution by a filtering membrane and storing the filtered extracting solution; online detection: identifying the hazardous waste substances in a stored product with an HPLC (high performance liquid chromatography)-TOF-MS (time-off-flight mass spectrometer). A first-level mass spectrum and a second-level mass spectrum can be fast and continuously scanned simultaneously in single once analytical determination by the HPLC-TOF-MS; the hazardous waste substances are identified by comparing acquired information with a database of the hazardous waste substances and comparing the second-level mass spectrum with a standard second-level mass spectrum, so that the resolution ratio is high, and the result accuracy is high.

The invention discloses a method suitable for detecting residues of eleven defoliating agents in cotton. The method is characterized by comprising the following steps: (1) preparing a sample solution to be detected, namely weighing cotton to be detected, and extracting by utilizing an accelerated solvent extraction device; by taking methanol as an extraction agent, operating according to a set extraction program; performing vacuum concentration after extraction is finished, fixing the volume and centrifuging; obtaining the supernatant; (2) preparing a standard solution, namely preparing a 0.01-0.30mu g/mL of gradient standard working solution of eleven defoliating agent pesticides; (3) injecting the gradient standard solution into an ultrahigh pressure liquid chromatography-tandem mass spectrometer, measuring in a positive and negative ion multiple-reaction monitoring mode, and making a standard curve equation; (4) measuring the supernatant obtained in the step (1) according to a method in the step (3) to finally obtain the content of each defoliating agent pesticide in the sample to be detected.

The invention provides a method for extracting and detecting rutin and quercetol, which is easy to realize automation, is environment-friendly, and has accurate and reliable measuring result and high sensitivity. The method adopts environment-friendly ionic liquid to replace poisonous organic solvent, and utilizes the high-temperature high-pressure condition in the accelerating solvent extraction technology to quickly extract active constituents such as rutin and quercetol in hawthorn of the traditional Chinese medicine, the extracted extract only needs to be simply processed and then can be directly transferred to a high performance liquid chromatograph separation system, and the processed extract can be detected by a chemiluminescence detector after being completely separated by a C18 column, the appearance condition is excellent, better detection result can be obtained, and the detection limit is low. The method can be used for detecting rutin and quercetol in foods, health products and other solid samples with very low content of rutin and quercetol.