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585 results about "Trichloroacetic acid" patented technology

Trichloroacetic acid (TCA; TCAA; also known as trichloroethanoic acid) is an analogue of acetic acid in which the three hydrogen atoms of the methyl group have all been replaced by chlorine atoms. Salts and esters of trichloroacetic acid are called trichloroacetates.

Method for simultaneously detecting multi-kind pesticide residues in bee products

InactiveCN101358953ASolve the problem of matrix effectFast wayComponent separationRetention timePhosphate
The present invention relates to a method of simultaneously detecting a plurality of agro-veterinary drug residues in bee products. The extracted liquid trichloroacetic acid or perchloric acid and the extracted liquid acetate, phosphate or borate solution are added into a sample; the pH value is controlled between 4.5 and 9.0; the mixed solution is centrifuged, the filtrate is added into a solid phase extraction column to be extracted, the extraction column is eluted and dried, the column is washed by oxalic acid-methanol solution, the volume of the eluent is defined by the aqueous solution of methanol, the eluent is added into liquid chromatography-tandem mass spectrometry to be analyzed and tested, the acquired chromatographic peak is contrasted with the known standard chromatographic peak of the drug, and according to the retention time and the abundance of the mass spectrum ions, the specific name of the detected drug is determined. The method only requires one pre-treatment of the sample, and thus can simultaneously extract 11 classes and more than 60 kinds of veterinary drug residues, such as sulfonamides, quinolones, macrolides, lincomycins, nitroimidazoles, beta-lactams, tetracyclines, chloromycetins, trinethoprims, chlordimeform, triadimenol and the like, the efficiency of analysis is high, and the detection cost is greatly reduced.
Owner:中华人民共和国江苏出入境检验检疫局

Separation and liquid chromatography column pre-column derivatization method of biogenic amine in soybean paste

The invention discloses a separation and liquid chromatography column pre-column derivatization method of biogenic amine in a soybean paste, comprising the following steps of: (1) adding a trichloroacetic acid solution to the soybean paste, homogenizing, centrifuging and collecting a supernate; (2) adding normal hexane to the supernate, vibrating and taking out a lower layer trichloroacetic acid phase for later use after static layering; (3) adding an NaOH solution to the trichloroacetic acid phase, then adding an NaHCO3 solution for buffering, and mixing in a dansyl chloride acetone solution to carry out derivatization; and (4) removing dansyl chloride to terminate the reaction to obtain a derivative solution and filtering. The separation method has simple treatment process and low reagent consumption and avoids analyte loss caused by transfer. The soybean paste can reach detection demands after being separated and purified; undesired peak disturbance of a spectrogram is less and the determinand loss is low, and the recovery rate of the biogenic amine can reach more than 80 percent. The method determines the optimum condition for deriving the biogenic amine; dansyl chloride derivative products are stable and the detection sensitivity is high.
Owner:NORTHEAST AGRICULTURAL UNIVERSITY

Method for detecting residual quantity of multiple polypeptidepolypeptide veterinary drugs in animal-derived food

The invention relates to the fields of analytical chemistry and food safety, particular to a method for detecting the residual quantity of multiple polypeptide veterinary drugs in animal-derived foods. The method comprises the following steps of: processing a sample with a TCA(trichloroacetic acid) and acetonitrile system for depositing proteins; extracting with a carbinol and 0.1% formic acid aqueous solution system; purifying with a Oasis HLB solid phase extraction column; performing gradient elution with an Eclipse XDB-C18 analytical column in the presence of an acetonitrile and 0.1% formic acid aqueous solution used as a mobile phase; and then performing electrospray and positive ion scanning mode separation for finally detecting four polypeptides. The limits of the four polypeptides, namely colistin, bacitracin A, polymyxin B and virginiamycin M, are 25 micrograms/kilogram, 100 micrograms/kilogram, 250 micrograms/kilogram and 120 micrograms/kilogram respectively; the recovery rates of colistin, bacitracin A, polymyxin B and virginiamycin M are 74.9-88.1%, 76.2-89.0%, 76.6-81.2% and 77.3-86.9% respectively; and the coefficients of variation (CV%) of colistin, bacitracin A, polymyxin B and virginiamycin M are 5.7-15.1%, 7.2-15.7%, 6.0-8.0% and 9.5-18.6% respectively. The detection limit, the recovery rate, the accuracy and other technical indexes all meet related detection requirements at home and aboard.
Owner:林维宣

Method for qualitatively and quantitatively analyzing histamine in muscles of miichthys miiuy by surface-enhanced Raman spectroscopy

The invention discloses a method for qualitatively and quantitatively analyzing histamine in muscles of miichthys miiuy by surface-enhanced Raman spectroscopy. The method comprises the following steps: mincing the muscles of the miichthys miiuy, making the minced muscles into minced meat, weighing certain parts of equivalent miichthys miiuy muscles to serve as samples, preparing histamine standard solutions of different concentrations, adding the histamine standard solutions into the samples, and using samples at different time points as labeling samples and prediction samples in a storage process; adding the labeling samples and the prediction samples into trichloroacetic acid, and filtering to obtain an extracting solution; measuring the histamine content of the miichthys miiuy meat of the prediction samples through HPLC (High Performance Liquid Chromatography); adding a nanometer enhancer into the extracting solution of the labeling samples, performing Raman spectrum data acquisition, and calculating corresponding Raman characteristic peaks of the histamine by a density functional theory; establishing a quantitative analysis model by using the peak intensity of the Raman characteristic peaks and the histamine content, and measuring the histamine concentration of the muscles of the miichthys miiuy by the quantitative analysis model. By adopting the method, the content of histamine of which the concentration is 1 to 150 mg/L in fresh fish can be detected accurately and quickly.
Owner:ZHEJIANG UNIV

Graphene-exfoliation hydrotalcite-like compound composite material immobilized protein modified electrode, production method and application thereof

The invention discloses a graphene (GR)-exfoliation hydrotalcite-like compound (ELDH) composite material immobilized protein modified electrode, a production method and an application thereof. The method comprises the following steps: compounding ELDH with negatively-charged exfoliation graphene oxide (GO) nanosheets through electrostatic attraction by using the characteristics of positive charges and large specific surface area of the ELDH, and reducing by using hydrazine hydrate to prepare a GR-ELDH hybrid; and sequentially immobilizing the GR-ELDH, ferrohemoglobin and chitosan on an ionic liquid modified carbon paste electrode through adopting a dispensing technology to produce the graphene-exfoliation hydrotalcite-like compound composite material immobilized protein modified electrode. The obtained modified electrode has monolayer GR nanosheet and ELDH synergistic effects, and the GR nanosheets increase the conductivity of the ELDH and inhibits the aggregation and accumulation of the ELDH; and the ELDH effectively inhibits the afresh stacking of the GR nanosheets, reduces the interlamellar contact resistance and improves the electron transfer rate of the above composite material, and a constructed CTS/GR-ELDH-Hb composite film-based third-generation trichloroacetic acid sensor has the advantages of low detection limit, wide detection range and small Michaelis constant.
Owner:徐州圣都金属科技有限公司

Milk and milk product tetracycline antibiotic residual quantity checking method

The invention relates to a method for detecting the residue amount of terracycline antibiotics in milk and dairy products. The method utilizes an ultra performance liquid chromatography - electrospray tandem triple quadrupole mass spectrometer to determine the residue amount of the terracycline antibiotics. The method is as follows: a sample is extracted from Na2EDTA-McIlvaine buffer solution (pH4.0); proteins are removed by trichloroacetic acids; a columella is extracted through an HLB solid phase and then purified and enriched; the sample is separated by a chromatographic column, with the column temperature of 30 DEG C; gradient elution is performed by utilization of water solution (v/v) which contains 0.1 percent of methanoic acids and acetonitrile as a moving phase; and quantitative detection is performed by adoption of the multi-reaction monitoring means. The detection limit of instruments is between 1.0 and 2.0 mu g/kg; a related coefficient r reaches over 0.999 within the linear range of between 1 and 100 mu g/kg; and the recovery rate is between 81.7 and 100.7 percent (the addition levels are 10 mu g/kg, 50 mu g/kg and 100 mu g/kg). The method has the advantages of quickness, accuracy, high sensitivity and wide application scope.
Owner:INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD

Method for extracting hirudin from leech saliva

The invention discloses a method for extracting hirudin form leech saliva. The method includes the following steps of a), placing leeches in a container to allow the leeches to be hungered sufficiently, inputting inductive substances to the leeches to allow the same to absorb fully, adding vomitives to allow the leeches to spit the saliva in bodies, taking out blood-sucking leech living bodies to return to a rearing pond to feed continuously, and meanwhile, collecting hirudin crude product liquid in the container; b), freezing above hirudin crude products, adding into precooled cold acetone, stirring prior to placing in a refrigerator for setting overnight, sucking supernatant acetone the next day prior to centrifuging, adding a trichloroacetic acid solution, and centrifuging to remove residues to obtain concentrated liquid; c), eluting the above concentrated liquid with an anion exchange column chromatography method, and performing gel filtration chromatography to obtain finished products. The method has the advantages of reasonable process, convenience and practicability in operation, good quality stability of the finished hirudin products and high yield, one-time pillage on the leeches with a traditional method can be avoided, wild resources of the leeches are protected, and development of leech farming is driven.
Owner:广西复鑫益生物科技有限公司

Preparation and catalytic application of Nafion/horseradish peroxidase/tricobalt tetraoxide-graphene/ionic liquid carbon paste electrode

The invention relates to a biosensor, particularly relates to a preparation method and catalytic application of a Nafion/horseradish peroxidase/tricobalt tetraoxide-graphene/ionic liquid carbon paste electrode (Nafion/HRP/Co3O4-GR/CILE) and belongs to the technical field of electrochemical analysis and detection. According to the preparation method of the Nafion/HRP/Co3O4-GR/CILE, an ionic liquid carbon paste electrode is used as a substrate electrode, and by virtue of the specific advantages of a Co3O4-GR nano composite material of large surface area and good biocompatibility, HRP is adsorbed on the surface of the material; and furthermore, the material is fixed by a Nafion film to prepare the Nafion/HRP/Co3O4-GR/CILE. HRP in the modified electrode keeps a natural structure and biological activity. Research on electrochemical properties of the modified electrode shows that the modified electrode has good electrochemical catalysis capability on trichloroacetic acid (TCA), and can be used for effectively detecting TCA, and the detection limit is 0.33mmol/L. The preparation method and the catalytic application, provided by the invention, do not cause environmental pollution; the modified electrode has good stability, repeatability and sensitivity, and the preparation process is simple, low in cost and easy to operate, so that the modified electrode has wide social benefits.
Owner:HAINAN NORMAL UNIV

A kind of enzyme-assisted extraction method of high-purity laver polysaccharide

The invention discloses an enzyme-assisted extraction method of high-purity laver polysaccharide, which belongs to the field of biomedicine. The seaweed is dried and ultrafinely pulverized to obtain seaweed powder, and the pulverized seaweed powder is subjected to supercritical CO2 extraction (extraction pressure is 31 MPa, temperature 50 ° C, extraction for 3 hours, separation pressure 5.6 MPa, temperature 55 ° C) degreased, and then The defatted seaweed powder was mixed with 50 times of pure water, 0.5% papain was added to extract at 70°C for 3.5 hours, the filter residue was discarded by centrifugation at 5000 rpm for 15 minutes, the extract was concentrated to 1/4 of the original volume by rotary evaporation, and 80% of Trichloroacetic acid (TCA) was mixed to 2% of the total volume of the solution, and then the solution was reacted in a 70°C water bath for 20 minutes to remove protein, centrifuged at 5000 rpm for 30 minutes to remove the precipitate, and dialyzed in deionized water for 48 hours to remove trichloroacetic acid. The dialysate was collected, and then Slowly add 4 times the volume of 95% ethanol, alcohol precipitation at 4°C for 12h, centrifuge at 5000rpm for 10min, discard the supernatant, wash the precipitate with absolute ethanol, acetone, and ether for three times, respectively, and dry it in an oven at 55°C. Seaweed crude polysaccharide. The yield of papain extraction technology was 26.07%, and the purity reached 84.32%. Compared with hot water extraction, the time was shortened by 50% and the yield was increased by 46%. The obtained laver polysaccharide can be widely used as the base material of medicine and health food.
Owner:NANJING UNIV OF FINANCE & ECONOMICS +1

Graphene-hydrotalcite-like compound-graphite phase carbon nitride composite material immobilized protein modified electrode, production method and application thereof

The invention discloses a graphene (GR)-hydrotalcite-like compound (LDH)-graphite phase carbon nitride (g-C3N4) composite material immobilized protein modified electrode, a production method and an application thereof. The method comprises the following steps: compounding an exfoliation hydrotalcite-like compound with negatively charged exfoliation graphene oxide nanosheets, mixing the obtained material with melamine, roasting, and adding water to recover in order to prepare a GR-LDH-g-C3N4 hybrid; and adding a GR-LDH-g-C3N4 and Hb mixed solution to an ionic liquid modified carbon paste electrode in a dropwise manner in order to produce the GR-LDH-g-C3N4 composite material immobilized protein modified electrode. The graphene-hydrotalcite-like compound-graphite phase carbon nitride composite material immobilized protein modified electrode fully displays advantages of a gel method and an integrating, merging and layering method, increases the specific surface area, the conductivity and the biocompatibility of the hybrid material, and inhibits the afresh stacking of GR sheets; and a roasting method allows g-C3N4 to grow on the surface of a GR sheet layer, increases the specific surface area of the hybrid material, and improves the electron transfer rate of an electrochemical reaction process. A constructed CTS / GR-LDH-g-C3N4-Hb composite film-based third-generation trichloroacetic acid sensor has the advantages of low detection limit, wide detection range and small Michaelis constant.
Owner:上海铭煦新材料有限公司

Extraction method of morindea officinalis polysaccharide

The invention provides an extraction method of morindea officinalis polysaccharide, belonging to the technical field of traditional Chinese medicines and solving the problems that in the existing morindea officinalis polysaccharide extraction method, the extraction method has complicated process steps and a poor protein removal effect, and the yield and purity of the obtained morindea officinalispolysaccharide are low. The extraction method of morindea officinalis polysaccharide in the invention comprises the following steps of: drying morindea officinalis rhizome and then smashing to 40-80 meshes; adding a chloroform/methanol mixed solvent in morindea officinalis powder for carrying out reflux extraction; carrying out alcohol extraction on a filter cake obtained by filtration and then adding water for lixiviation; subsequently, filtering and concentrating a filtrate, carrying out alcohol precipitation on a concentrated liquid and then filtering so as to obtain the crude morindea officinalis polysaccharide; adding the crude morindea officinalis polysaccharide into a n-butanol/trichloroacetic acid mixed solvent for processing, and entering a chromatographic column for elution; andcarrying out concentration, alcohol precipitation, filtration and drying on an effluent liquid so as to obtain the morindea officinalis polysaccharide. The extraction method of the morindea officinalis polysaccharide in the invention has a simple process and a good protein removal effect, and the extracted morindea officinalis polysaccharide has less impurities and high yield and purity.
Owner:朱孟勇

Detection method for galacto-oligosaccharide based on biological enzyme technology

The invention provides a detection method for galacto-oligosaccharide based on biological enzyme technology, which belongs to the technical field of food engineering. According to the invention, at first, the method of removing proteins by using trichloroacetic acid and lead acetate is employed for pretreatment of an object to be detected, and membrane filtration is utilized to remove impurities so as to obtain a sample to be detected; then, sodium hydroxide and sodium acetate with different concentration are utilized for ion exchange and gradient elution; finally, a four-potential pulsed amperometric detector is used for detection. The invention is applicable to separation and detection of cow's milk containing galacto-oligosaccharide and a variety of galacto-oligosaccharide components in a galacto-oligosaccharide solution system; employment of ion chromatography, utilization of the methods of ion exchange and gradient elution for separation of galacto-oligosaccharide and cooperativedetection with the four-potential pulsed amperometric detector enable contamination and interference to an analytical column, the detector and the like caused by macro-molecular substances such as proteins, fat and emulsifiers which might exist in the sample to be eliminated, thereby allowing accurate and rapid detection to be achieved.
Owner:SHANGHAI JIAO TONG UNIV
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