CN101750242A - Sample pretreatment method for detecting harmful substances in meat product and aquatic product - Google Patents
Sample pretreatment method for detecting harmful substances in meat product and aquatic product Download PDFInfo
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- CN101750242A CN101750242A CN200810182577A CN200810182577A CN101750242A CN 101750242 A CN101750242 A CN 101750242A CN 200810182577 A CN200810182577 A CN 200810182577A CN 200810182577 A CN200810182577 A CN 200810182577A CN 101750242 A CN101750242 A CN 101750242A
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Abstract
The invention discloses a sample pretreatment method for detecting harmful substances in a meat product and an aquatic product, which comprises the following steps of firstly, wringing a meat sample or a fish sample; secondly, extracting by adding extraction solvent and obtaining filtrate by filtering extract; thirdly, selectively adsorbing and removing proteins, polypeptide, amino acid and fatty substances in the filtrate by utilizing adsorption materials which can remove the proteins, the polypeptide, the amino acid and fats; and fourthly, centrifugation, carrying out centrifugal separation on the sample experiencing the steps from one to three, and taking supernatant for further analysis and detection or for further analysis and detection after concentration. The invention can be used for analysis and detection of a plurality of kinds of chemical compositions in the meat product and the aquatic product and has the advantages of rapidness, strong universality and the like.
Description
Technical field
The present invention relates to the food hygiene detection field, especially relate to the sample pretreating method that is used for detecting meat products and aquatic products objectionable impurities.
Background technology
Analyzing and testing for harmful chemical in food or the agricultural product, no matter use which kind of analyzing detecting method, usually all need analyzed microchemistry composition is separated preferably with sample main matrix (as protein, fat, starch and pigment etc.) and other impurity, to avoid the interference of matrix for detection accuracy.Normally used method comprises albumen precipitation, liquid-liquid extraction and Solid-Phase Extraction etc.Speed is slow, the defective of versatility difference but present detection method has.
Along with the Food Inspection growth of requirement, be necessary the further more simple and reliable method of exploitation.Particularly meat products and aquatic products, as the big series products of one in the food, the source disperses extensively, be necessary to develop a kind of fast, the detection meat products The pretreatment method of highly versatile.Be beneficial to analyzing and testing accurately.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of sample pretreating method that is used for detecting meat products and aquatic products objectionable impurities.This sample pretreating method can be used for analyzing and detecting various chemical components in meat products and the aquatic products, be a kind of fast, the sample pretreating method of highly versatile.
For solving the problems of the technologies described above, the present invention is used for detecting the sample pretreating method of meat and aquatic products objectionable impurities, comprises the steps:
1) meat sample or flesh of fish sample are rubbed;
2) adding the extraction solvent extracts; Extracting liquid filtering obtains filtrate;
3) utilize the sorbing material that can remove deproteinize, polypeptide, amino acid and fat from filtrate, optionally to adsorb and remove deproteinize, polypeptide, amino acid and fatty material;
4) centrifugal, will finish above-mentioned all step 1)-3) sample carry out centrifuging, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
1-the present invention is used for detecting the sample pretreating method of meat and aquatic products objectionable impurities, and alkalescence or neutral organic substance in analyzing and testing meat and aquatic products comprise the steps:
1) meat sample or flesh of fish sample are rubbed;
2) adding acidic aqueous solution or acidic organic solvent or organic solvent extracts; Extracting liquid filtering obtains filtrate;
3) in filtrate, add the sorbing material that can remove deproteinize, polypeptide, amino acid and fat;
4) centrifugal, will finish above-mentioned all step 1)-3) sample carry out centrifuging, get supernatant and be used for progressive analyzing and testing or after concentrated, further carry out analyzing and testing.
Step 2) acidic aqueous solution in can be but be not limited to the potpourri that a kind of in the following kind or several arbitrary proportion mix:
The aqueous solution of trichloroacetic acid, sulfosalicylic acid, hydrochloric acid, trifluoroacetic acid, formic acid, acetate, nitric acid, phosphoric acid, perchloric acid.The concentration (weight ratio) of acid is between 0.01% to 10%.
Further improved technical scheme, step 2) acidic aqueous solution in can contain the water-soluble organic solvent of energy, operable organic solvent has, but is not limited to: methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran.People with relevant professional knowledge can use the water-soluble organic solvent of many similar energy according to above explanation.Similarly organic solvent can't exclusive list, but should belong to fundamental spirit of the present invention, belongs to the row of the present invention's protection.The content of organic solvent (volume ratio) can from 1% to 99%.
Step 2) also can use pure organic solvent in or contain sour organic solvent as extract.Operable organic solvent has, but is not limited to: methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran.The acid of using can be the potpourri that a kind of of following acid or several arbitrary proportion mix: trichloroacetic acid, sulfosalicylic acid, hydrochloric acid, trifluoroacetic acid, formic acid, acetate, nitric acid, phosphoric acid, perchloric acid.The concentration (weight ratio) of acid is between 0.01% to 10%.
Sorbing material in the step 3) is to have alkalescence and lipophilic any or several compound substance simultaneously, or the potpourri of alkaline sorbing material and lipophilicity sorbing material.Material can be superpolymer or its finishing thing, or the bonded silica gel material.Its instantiation has, but is not limited to: the polystyrene copolymerization divinylbenzene resin that various amination polystyrene copolymerization divinylbenzene resins, quaternary ammonium salt replace, contain the polystyrene copolymerization divinylbenzene resin of following basic functionality: pyridine, pyrrole is pressed against, pyrans, 1,4 cyclohexanediamine.Described material also can be the high polymer material that contains amino, quaternary ammonium salt or above any one or several alkaline organo-functional group.Described material also can be the bonded silica gel material that contains amino, quaternary ammonium salt or above any one or several alkaline organo-functional group, as but be not limited to: aminopropyl silica gel, quaternary ammonium group propyl group silica gel.Following material can be used as the lipophilicity sorbing material in the potpourri of alkaline sorbing material and lipophilicity sorbing material: octadecyl silane, octane bonded silica gel, dodecyl bonded silica gel, this resin of polystyrene copolymerization divinyl.Based on core spirit of the present invention, the professional with relevant knowledge can enumerate many similar lipophilicity polymeric adsorbents, and these materials all belong to the protection domain of this invention.
As further improvement in the technical proposal, the particle size range of described sorbing material is 0.1 micron～5 millimeters, and specific surface area is 10～800 square meter/grams, and average pore size is 5～100 nanometers.Degree of substitution is 0.3-3.5 mM/gram.
As further improvement in the technical proposal, before adding sorbing material, can add aqueous slkali with neutralizing acid in the extract after acidic extraction.
The present invention can be used for various meats and aquatic products; The present invention also can be used for freezing pork, the freezing flesh of fish, cooked meat product and canned meat, canned fish or other similar meat products; Also can be used for all kinds of freezing pork, beef and muttons, stewed meat products, sauce fish product, the meat products that fire-cures, smoked fish goods, smoked boiled sausage goods, the smoked relevant goods with meat and aquatic products such as cooked meat products such as ham product, pickle cured meat product, cattle and sheep meat, Pork and meat of poultris can that boil.
Adopt the sample of the resultant purification of the present invention further to use, carry out analyzing and testing but be not limited to following method: vapor-phase chromatography, gas chromatography-mass spectrography, liquid phase chromatography, liquid chromatograph mass spectrography, Capillary Electrophoresis, enzyme reagent immunodetection, various direct spectrum detection methods.
The chemical substance composition that is used for testing after purifying through method of the present invention comprises a class or a few class of following material: molecular weight is not higher than 2000 daltonian organic amines, nitrogenous organic heterocyclic compounds, amide-type, oxygen containing organic heterocyclic compounds, ether compound, various alcohol compound.Concrete chemical substance composition example as: melamine, aminoglycoside medicaments, Clenbuterol and various alkaline stimulant substance have the microbiotic of alkalescence etc.Also comprise various negative ion through the chemical substance composition that is used to test after the method purification of the present invention.
2-the present invention is used for detecting the sample pretreating method of meat and aquatic products objectionable impurities, and the acid or neutral organic substance in analyzing and testing meat and aquatic products comprises the steps:
1) meat sample or flesh of fish sample are rubbed;
2) organic solvent that adds alkaline aqueous solution or alkalescence extracts; Filtration obtains filtrate
3) in filtrate, add the sorbing material that can remove deproteinize, polypeptide, amino acid and fat;
4) centrifugal, will finish above-mentioned all step 1)-3) sample carry out centrifuging, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
Step 2) alkaline aqueous solution in can be but be not limited to the potpourri that a kind of in the following kind or several arbitrary proportion mix:
The aqueous solution of ammoniacal liquor, triethylamine, NaOH, sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, sodium dihydrogen phosphate.The concentration of alkali (weight ratio) is between 0.01% to 10%
Further improved technical scheme, step 2) alkaline aqueous solution in can contain the water-soluble organic solvent of energy, operable organic solvent has, but is not limited to: methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran.People with relevant professional knowledge can use many similar organic solvents according to above explanation.Similarly organic solvent can't exclusive list, but should belong to fundamental spirit of the present invention, belongs to the row of the present invention's protection.The content of organic solvent (volume ratio) can from 1% to 99%.
The organic solvent that also can use pure organic solvent step 2) or contain alkali is as extract.Operable capable machine solvent has, but is not limited to: methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran.The alkali that uses can be a kind of of following alkali or several potpourri: the aqueous solution of ammoniacal liquor, triethylamine, NaOH, sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, sodium dihydrogen phosphate.The concentration of alkali (weight ratio) is between 0.01% to 10%.
Sorbing material in the step 3) is to have acid and lipophilic any or several compound substance simultaneously, or the potpourri of acid sorbing material and lipophilicity sorbing material.Material can be superpolymer or its finishing thing, or the bonded silica gel material.Its instantiation has, but is not limited to: various sulfonated polystyrene copolymerization divinylbenzene resins, carboxylic polystyrene copolymerization divinylbenzene resin.Described material also can be the high polymer material that contains sulfonic group, carboxyl or any one or several acid organo-functional group.Described material also can be the bonded silica gel material that contains sulfonic group, carboxyl or any one or several acid organo-functional group.Following material can be used as the lipophilicity sorbing material in the potpourri of acid sorbing material and lipophilicity sorbing material: octadecyl silane, octane bonded silica gel, dodecyl bonded silica gel, this resin of polystyrene copolymerization divinyl.Based on core spirit of the present invention, the professional with relevant knowledge can enumerate many similar lipophilicity polymeric adsorbents, and these materials all belong to the protection domain of this invention.
As further improvement in the technical proposal, the particle size range of described sorbing material is 0.1 micron～5 millimeters, and specific surface area is 10～800 square meter/grams, and average pore size is 5～100 nanometers.Degree of substitution is at 0.3-3.5 mM/gram.
As further improvement in the technical proposal, before adding polymeric adsorbent, can in the extract after alkalescence is extracted, add acid solution with neutralization bases.
The present invention can be used for various meats and aquatic products; The present invention also can be used for freezing pork, the freezing flesh of fish, cooked meat product and canned meat, canned fish or other similar meat products; Also can be used for all kinds of freezing pork, beef and muttons, stewed meat products, sauce fish product, the meat products that fire-cures, smoked fish goods, smoked boiled sausage goods, the smoked relevant goods with meat and aquatic products such as cooked meat products such as ham product, pickle cured meat product, cattle and sheep meat, Pork and meat of poultris can that boil.
Adopt the sample of the resultant purification of the present invention further to use, carry out analyzing and testing but be not limited to following method: vapor-phase chromatography, gas chromatography-mass spectrography, liquid phase chromatography, liquid chromatograph mass spectrography, Capillary Electrophoresis, enzyme reagent immunodetection, various direct spectrum detection methods.
The class or a few class that comprise following material through the chemical substance composition that is used for testing after the method purification of the present invention: molecular weight is not higher than 2000 daltonian organic acids, amide-type, oxygen containing organic heterocyclic compounds, ether compound, various alcohol compound.Concrete chemical substance composition example is as cyanuric acid, salicylic acid microbiotic etc.Also comprise each metal ion species through the chemical substance composition that is used to test after the method purification of the present invention.
Be used for detecting the sample treatment of meat products and aquatic products objectionable impurities, the mode of removing deproteinize, polypeptide, amino acid and fat comprises: directly adding can remove deproteinize, polypeptide, amino acid and fatty sorbing material in filtrate; Or with filtrate by containing the sorbing material that can remove deproteinize, polypeptide, amino acid and fat.Filtrate is by containing the sorbing material that can remove deproteinize, polypeptide, amino acid and fat, and the mode that can adopt includes, without being limited to filtrate by being filled with the duckpin of sorbing material; With filtrate by being filled with the syringe filter of sorbing material; With filtrate by being filled with the liquid-transfering gun head of sorbing material; With filtrate by containing the filtering membrane of sorbing material.
The present invention can be used for analyzing and detecting various chemical components in the meat products, has fast, advantage such as highly versatile.
Embodiment
Complete sample purification process of the present invention mainly comprises following mode:
Alkalescence or neutral organic substance in 1-analyzing and testing meat and the aquatic products
Comprise the steps:
Meat sample or flesh of fish sample are rubbed, adding acidic aqueous solution or acidic organic solvent extracts, extracting liquid filtering, obtain filtrate, in filtrate, add the sorbing material that can remove deproteinize, polypeptide, amino acid and fat, mix the back centrifuging, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
Acid or neutral organic substance in 2-analyzing and testing meat and the aquatic products
Comprise the steps:
Meat sample or flesh of fish sample are rubbed, the organic solvent that adds alkaline aqueous solution or alkalescence extracts, extracting liquid filtering, obtain filtrate, in filtrate, add the sorbing material that can remove deproteinize, polypeptide, amino acid and fat, mix the back centrifuging, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
Embodiment 1
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 0.01% trichloroacetic acid solution 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 0.01% trichloroacetic acid solution; Adding particle diameter in filtrate is 0.1 micron, and specific surface area is 10 square meter/grams, and average pore size is the various amination polystyrene copolymerization divinylbenzene resin 1g of 5 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 2
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add acid concentration (weight ratio) and be the aqueous solution 15mL of 0.5% sulfosalicylic acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Hold to 25mL with 0.5% sulfosalicylic acid; Adding particle diameter in filtrate is 300 microns, and specific surface area is 60 square meter/grams, and average pore size is the polystyrene copolymerization divinylbenzene resin 1g that the quaternary ammonium salt of 11 nanometers replaces; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 3
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 1% aqueous hydrochloric acid solution 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 1% aqueous hydrochloric acid solution; Adding particle diameter in filtrate is 600 microns, and specific surface area is 110 square meter/grams, average pore size be 17 nanometers contain pyridine radicals polystyrene copolymerization divinylbenzene resin (degree of substitution=1.8 mM/grams) 1g; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 4
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 1.5% trifluoroacetic acid aqueous solution 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 1.5% trifluoroacetic acid aqueous solution; Adding particle diameter in filtrate is 900 microns, and specific surface area is 160 square meter/grams, and average pore size is that the pyrrole of 23 nanometers is pressed against base polystyrene copolymerization divinylbenzene resin (degree of substitution=2.8 Bo moles per gram) 1g; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 5
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 2% aqueous formic acid 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 2% aqueous formic acid; Adding particle diameter in filtrate is 1200 microns, and specific surface area is 200 square meter/grams, and average pore size is pyranose polystyrene copolymerization divinylbenzene resin (degree of substitution=0.4 mM/gram) 1g of 29 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 6
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 2.5% acetic acid aqueous solution 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 2.5% acetic acid aqueous solution; Adding particle diameter in filtrate is 1560 microns, and specific surface area is 250 square meter/grams, and average pore size is 1,4 cyclohexanediamine base polystyrene copolymerization divinylbenzene resin (degree of substitution=0.8 mM/gram) 1g of 35 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 7
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 3% aqueous solution of nitric acid 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 3% aqueous solution of nitric acid; Adding particle diameter in filtrate is 1870 microns, and specific surface area is 300 square meter/grams, and average pore size is aminomethyl polystyrene-divinylbenzene (degree of substitution=1.2 mM/grams) 1g of 41 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 8
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 3.5% phosphate aqueous solution 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 3.5% phosphate aqueous solution; Adding particle diameter in filtrate is 2200 microns, and specific surface area is 360 square meter/grams, and average pore size is the N of 47 nanometers, N, N trimethyl aminomethyl polystyrene-divinylbenzene (degree of substitution 2.8 mM/grams) 1g, octadecyl silane (carbon content is 17%, percentage by weight) 1 gram; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 9
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 4% high chloro acid solution 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 4% high chloro acid solution; Adding particle diameter in filtrate is 2500 microns, and specific surface area is 400 square meter/grams, and average pore size is aminopropyl bonded silica gel (carbon content is 6%, the percentage by weight) 1g of 53 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 10
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the trichloroacetic acid that contains methyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the trichloroacetic acid that contains methyl alcohol is settled to 25mL; Adding particle diameter in filtrate is 2800 microns, and specific surface area is 450 square meter/grams, and average pore size is the N of 59 nanometers, N, N trimethyl aminopropyl bonded silica gel (carbon content is 9%, percentage by weight) 1g; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the trichloroacetic acid of methyl alcohol, its sour concentration (weight ratio) is 4.5%, the content of methyl alcohol (volume ratio) is 1%.
Embodiment 11
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the sulfosalicylic acid that contains ethanol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the sulfosalicylic acid that contains ethanol is settled to 25mL; Adding particle diameter in filtrate is 3100 microns, and specific surface area is 510 square meter/grams, and average pore size is the aminopropyl silica gel 1g of 65 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the sulfosalicylic acid of ethanol, its sour concentration (weight ratio) is 5%, the content of methyl alcohol (volume ratio) is 13%.
Embodiment 12
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add the aqueous solution of hydrochloric acid 15mL that contains propyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with the aqueous solution of hydrochloric acid that contains propyl alcohol; Adding particle diameter in filtrate is 3400 microns, and specific surface area is 560 square meter/grams, and average pore size is the quaternary ammonium group propyl group silica gel 1g of 71 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution of hydrochloric acid that contains propyl alcohol, its sour concentration (weight ratio) is 5.5%, the content of methyl alcohol (volume ratio) is 25%.
Embodiment 13
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the trifluoroacetic acid that contains isopropyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the trifluoroacetic acid that contains isopropyl alcohol is settled to 25mL; Adding particle diameter in filtrate is 3700 microns, and specific surface area is 610 square meter/grams, and average pore size is the octadecyl silane 1g of 77 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the trifluoroacetic acid of isopropyl alcohol, its sour concentration (weight ratio) is 6%, the content of methyl alcohol (volume ratio) is 37%.
Embodiment 14
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the formic acid that contains butanols, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the formic acid that contains butanols is settled to 25mL; Adding particle diameter in filtrate is 4000 microns, and specific surface area is 660 square meter/grams, and average pore size is the octane bonded silica gel 1g of 83 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the formic acid of butanols, its sour concentration (weight ratio) is 6.5%, the content of methyl alcohol (volume ratio) is 49%.
Embodiment 15
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add the acetic acid water solution 15mL that contains isobutyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with the acetic acid water solution that contains isobutyl alcohol; Adding particle diameter in filtrate is 4400 microns, and specific surface area is 710 square meter/grams, and average pore size is the dodecyl bonded silica gel 1g of 89 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned acetic acid water solution that contains isobutyl alcohol, its sour concentration (weight ratio) is 7%, the content of methyl alcohol (volume ratio) is 61%.
Embodiment 16
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the nitric acid that contains acetonitrile, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the nitric acid that contains acetonitrile is settled to 25mL; Adding particle diameter in filtrate is 4700 microns, and specific surface area is 760 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 95 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the nitric acid of acetonitrile, its sour concentration (weight ratio) is 7.5%, the content of methyl alcohol (volume ratio) is 73%.
Embodiment 17
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the phosphoric acid that contains acetone, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the phosphoric acid that contains acetone is settled to 25mL; Adding particle diameter in filtrate is 4700 microns, and specific surface area is 760 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 95 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the phosphoric acid of acetone, its sour concentration (weight ratio) is 8%, the content of methyl alcohol (volume ratio) is 85%.
Embodiment 18
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the perchloric acid that contains tetrahydrofuran, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the perchloric acid that contains tetrahydrofuran is settled to 25mL; Adding particle diameter in filtrate is 4700 microns, and specific surface area is 760 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 95 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) get that supernatant is used for further analyzing and testing or through concentrating the laggard stepping analyzing and testing of spreading out.The above-mentioned aqueous solution that contains the perchloric acid of tetrahydrofuran, its sour concentration (weight this) is 9%, the content of methyl alcohol (volume ratio) is 97%.
Embodiment 19
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add methyl alcohol 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; With methanol constant volume to 25mL; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 20
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add ethanol 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with ethanol; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got the liquid that disappears and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 21
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add propyl alcohol 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with propyl alcohol; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 22
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add isopropyl alcohol 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with isopropyl alcohol; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 23
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add butanols 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with butanols; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 24
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add isobutyl alcohol 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with isobutyl alcohol; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for progressive analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 25
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add acetonitrile 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with acetonitrile; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 26
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add acetone 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with acetone; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 27
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add tetrahydrofuran 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with tetrahydrofuran; Adding particle diameter in filtrate is 5000 microns, and specific surface area is 800 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 100 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 28
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 10% the methanol solvate 15mL that contains trichloroacetic acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Be settled to 25mL with 10% methanol solvate that contains trichloroacetic acid; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 29
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 9% the alcohol solvent 15mL that contains sulfosalicylic acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Alcohol solvent with 9% sulfosalicylic acid is settled to 25mL; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 30
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 8% hydrochloric propyl alcohol solvent 15mL, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Propyl alcohol solvent with 8% hydrochloric acid is settled to 25mL; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 31
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 7% the isopropanol solvent 15mL that contains trifluoroacetic acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Isopropanol solvent with 7% trifluoroacetic acid is settled to 25mL; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 32
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 60% the butanols solvent 15mL that contains formic acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Butanols solvent with 6% formic acid is settled to 25mL; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 33
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 5% the iso-butanol solvent 15mL that contains acetate, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Iso-butanol solvent with 5% acetate is settled to 25mL; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 34
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 1% the fine solvent 15mL of the second that contains nitric acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Second eyeball solvent with 1% nitric acid is settled to 25mL; Adding particle diameter in filtrate is 3000 microns, and specific surface area is 360 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 48 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 35
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add acid concentration (weight ratio) and be the acetone solvent 15mL of 0.1% phosphoric acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Acetone solvent with 0.1% phosphoric acid is settled to 25mL; Adding particle diameter in filtrate is 1500 microns, and specific surface area is 200 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 30 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 36
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 0.01% the tetrahydrofuran solvent 15mL that contains perchloric acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Tetrahydrofuran solvent with 0.01% perchloric acid is settled to 25mL; Adding particle diameter in filtrate is 3400 microns, and specific surface area is 560 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 70 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or carry out analyzing and testing through concentrating the laggard step.
Embodiment 37
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Adding acid concentration (weight ratio) is 0.01% the tetrahydrofuran solvent 15mL that contains perchloric acid, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Add the ammoniacal liquor neutralizing acid in the filtrate; Be settled to 25mL with tetrahydrofuran; Adding particle diameter in filtrate is 3400 microns, and specific surface area is 560 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 70 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 38
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 0.01% ammoniacal liquor, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 0.01% ammoniacal liquor is settled to 25mL; Adding particle diameter in filtrate is 0.1 micron, and specific surface area is 10 square meter/grams, and average pore size is the various sulfonated polystyrene copolymerization divinylbenzene resin 1g of 5 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 39
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 0.5% triethylamine, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 0.5% triethylamine is settled to 25mL; Adding particle diameter in filtrate is 300 microns, and specific surface area is 60 square meter/grams, and average pore size is the carboxylic polystyrene copolymerization divinylbenzene resin 1g of 11 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 40
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 1% NaOH, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 1% NaOH is settled to 25mL; Adding particle diameter in filtrate is 600 microns, and specific surface area is 110 square meter/grams, and average pore size is sulfonic group polystyrene-divinylbenzene (degree of substitution=3.0 mM/grams) 1g of 17 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 41
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 1.5% sodium carbonate, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 1.5% sodium carbonate is settled to 25mL; Adding particle diameter in filtrate is 900 microns, and specific surface area is 160 square meter/grams, and average pore size is carboxy-functionalized polystyrene-divinylbenzene (degree of substitution=0.6 mM/gram) 1g of 23 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 42
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 2% sodium bicarbonate, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 2% sodium bicarbonate is settled to 25mL; Adding particle diameter in filtrate is 1200 microns, and specific surface area is 200 square meter/grams, and average pore size is that the acid organo-functional group benzene sulfonic acid base key of 29 nanometers closes silica gel (degree of substitution=0.3 mM/gram) 1g; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 43
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 2.5% sodium acetate, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 2.5% sodium acetate is settled to 25mL; Adding particle diameter in filtrate is 1560 microns, and specific surface area is 250 square meter/grams, and average pore size is acid organo-functional group carboxyl bonded silica gel (degree of substitution=0.6 mM/gram) 1g of 35 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 44
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 3% sodium phosphate, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 3% sodium phosphate is settled to 25mL; Adding particle diameter in filtrate is 1870 microns, and specific surface area is 300 square meter/grams, and average pore size is the octadecyl silane 1g of 41 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 45
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; Add alkali concn (weight ratio) and be the aqueous solution 15mL of 3.5% sodium dihydrogen phosphate, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with 3.5% sodium dihydrogen phosphate is settled to 25mL; Adding particle diameter in filtrate is 2200 microns, and specific surface area is 360 square meter/grams, and average pore size is the octane bonded silica gel 1g of 47 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got the liquid that disappears and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.
Embodiment 46
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the ammoniacal liquor that contains methyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the ammoniacal liquor that contains methyl alcohol is settled to 25mL; Adding particle diameter in filtrate is 2800 microns, and specific surface area is 450 square meter/grams, and average pore size is the dodecyl bonded silica gel 1g of 59 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the ammoniacal liquor of methyl alcohol, its sour concentration (weight ratio) is 4.5%, the content of methyl alcohol (volume ratio) is 1%.
Embodiment 47
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the triethylamine that contains ethanol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the triethylamine that contains ethanol is settled to 25mL; Adding particle diameter in filtrate is 3100 microns, and specific surface area is 510 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 65 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the triethylamine of ethanol, its sour concentration (weight ratio) is 5%, the content of methyl alcohol (volume ratio) is 13%.
Embodiment 48
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the NaOH that contains propyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the NaOH that contains propyl alcohol is settled to 25mL; Adding particle diameter in filtrate is 3400 microns, and specific surface area is 560 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 71 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the NaOH of propyl alcohol, its sour concentration (weight ratio) is 5.5%, the content of methyl alcohol (volume ratio) is 25%.
Embodiment 49
Be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps:
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the sodium carbonate that contains isopropyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Aqueous solution with the sodium carbonate that contains isopropyl alcohol is settled to 25mL; Adding particle diameter in filtrate is 3700 microns, and specific surface area is 610 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 77 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the sodium carbonate of isopropyl alcohol, its sour concentration (weight ratio) is 6%, the content of methyl alcohol (volume ratio) is 37%.
Embodiment 50
Meat sample or flesh of fish sample are rubbed, take by weighing sample 1g; The aqueous solution 15mL that adds the sodium carbonate that contains isopropyl alcohol, ultrasonic Extraction 10 minutes; Filtration obtains filtrate; Add the hydrochloric acid neutralization bases in the filtrate; Water is settled to 25mL; Adding particle diameter in filtrate is 3700 microns, and specific surface area is 610 square meter/grams, and average pore size is this resin of polystyrene copolymerization divinyl 1g of 77 nanometers; Centrifugal behind the whirlpool mixing (10000RPM, 5 minutes) are got supernatant and are used for further analyzing and testing or further carry out analyzing and testing after concentrating.The above-mentioned aqueous solution that contains the sodium carbonate of isopropyl alcohol, its sour concentration (weight ratio) is 6%, the content of methyl alcohol (volume ratio) is 37%.
Embodiment 51
The present invention is used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, comprise the steps: to take by weighing sample 1g, add 0.1mol/L hydrochloric acid 15mL, add 60g/L sulfosalicylic acid 3mL behind the ultrasonic Extraction 10min, be settled to 25mL, add polystyrene copolymerization divinylbenzene resin 1g and octadecyl silane 1g that quaternary ammonium salt replaces with 0.1mol/L hydrochloric acid, centrifugal (10000RPM behind the whirlpool mixing, 5 minutes), get supernatant and cross film, use for liquid chromatographic detection.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (21)
1. be used for detecting the sample pretreating method of meat products and aquatic products objectionable impurities, it is characterized in that, comprise the steps:
1) meat sample or flesh of fish sample are rubbed;
2) adding the extraction solvent extracts; Extracting liquid filtering obtains filtrate;
3) utilize the sorbing material that can remove deproteinize, polypeptide, amino acid and fat from filtrate, optionally to adsorb and remove deproteinize, polypeptide, amino acid and fatty material;
4) centrifugal, will finish above-mentioned all step 1)-3) sample carry out centrifuging, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
2. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 1, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, meat sample or flesh of fish sample are rubbed, adding acid solution or organic solvent extracts, extracting liquid filtering obtains filtrate, utilization can remove deproteinize, polypeptide, the sorbing material of amino acid and fat optionally adsorbs from filtrate except that deproteinize, polypeptide, amino acid and fatty material, centrifugal, carry out centrifuging with finishing above-mentioned sample in steps, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
3. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 1, it is characterized in that: the acid or neutral organic substance in described analyzing and testing meat and the aquatic products, meat sample or flesh of fish sample are rubbed, adding alkaline solution or organic solvent extracts, extracting liquid filtering obtains filtrate, utilization can remove deproteinize, polypeptide, the sorbing material of amino acid and fat optionally adsorbs from filtrate except that deproteinize, polypeptide, amino acid and fatty material, centrifugal, carry out centrifuging with finishing above-mentioned sample in steps, get supernatant and be used for further analyzing and testing or after concentrating, further carry out analyzing and testing.
4. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 2, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, the acid solution that adds extracts, the aqueous solution that described acid solution comprises trichloroacetic acid, sulfosalicylic acid, hydrochloric acid, trifluoroacetic acid, formic acid, acetate, nitric acid, phosphoric acid, perchloric acid is a kind of or several arbitrary proportion mixes.
5. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 4, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, the acidic aqueous solution that adds extracts, and can contain in the described acid solution to comprise methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran by water-soluble organic solvent.
6. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 5, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, add acidic aqueous solution and extract, the content (volume ratio) that contains organic solvent that can be water-soluble in the described acidic aqueous solution is 1% to 99%.
7. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 2, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, the acid solution that adds extracts, and described acid solution comprises methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran organic solvent; The solvent that the acid of using comprises trichloroacetic acid, sulfosalicylic acid, hydrochloric acid, trifluoroacetic acid, formic acid, acetate, nitric acid, phosphoric acid, perchloric acid is a kind of or several arbitrary proportion mixes.
8. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 2, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, add acid solution and extract, the concentration (weight ratio) from 0.01% to 10% of acid in the described acid solution.
9. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 3, it is characterized in that: the acid or neutral organic substance in described analyzing and testing meat and the aquatic products, the alkaline solution that adds extracts, the aqueous solution that described alkaline solution comprises ammoniacal liquor, triethylamine, NaOH, sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, sodium dihydrogen phosphate is a kind of or several arbitrary proportion mixes.
10. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 9, it is characterized in that: the acid or neutral organic substance in described analyzing and testing meat and the aquatic products, the alkaline aqueous solution that adds extracts, and can contain in the described alkaline aqueous solution to comprise methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran by water-soluble organic solvent.
11. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 3, it is characterized in that: the acid or neutral organic substance in described analyzing and testing meat and the aquatic products, the alkaline solution that adds extracts, and described alkaline solution comprises methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran organic solvent; The solvent that the alkali that uses comprises ammoniacal liquor, triethylamine, NaOH, sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, sodium dihydrogen phosphate is a kind of or several arbitrary proportion mixes.
12. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 3, it is characterized in that: the acid or neutral organic substance in described detection meat and the aquatic products, add alkaline solution and extract the concentration of alkali (weight ratio) from 0.01% to 10% in the described alkaline solution.
13. the sample extraction method that is used for detecting meat products and aquatic products objectionable impurities according to claim 1 is characterized in that: described extraction solvent can be that organic solvent comprises methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutyl alcohol, acetonitrile, acetone, tetrahydrofuran.
14. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 2, it is characterized in that: alkalescence or neutral organic substance in described analyzing and testing meat and the aquatic products, the employed sorbing material that removes deproteinize, polypeptide, amino acid and fat, described sorbing material can be to have alkalescence and lipophilic any or several compound substance simultaneously, or the potpourri of alkaline sorbing material and lipophilicity sorbing material.
15. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 14, it is characterized in that: described have alkalescence and lipophilic any or several compound substance simultaneously, this material can be superpolymer or its finishing thing, or bonded silica gel material, comprise the polystyrene copolymerization divinylbenzene resin that various amination polystyrene copolymerization divinylbenzene resins, quaternary ammonium salt replace, the polystyrene copolymerization divinylbenzene resin that contains following basic functionality: pyridine, pyrrole are pressed against, pyrans, 1,4 cyclohexanediamine; Described material also can be the high polymer material that contains amino, quaternary ammonium salt or above any one or several alkaline organo-functional group; Described material also can be the bonded silica gel material that contains amino, quaternary ammonium salt or above any one or several alkaline organo-functional group, aminopropyl silica gel, quaternary ammonium group propyl group silica gel.
16. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 14, it is characterized in that: the potpourri of described alkaline sorbing material and lipophilicity sorbing material, this mixture material can be superpolymer or its finishing thing, or bonded silica gel material, the lipophilicity sorbing material that can be used as in the potpourri of alkaline sorbing material and lipophilicity sorbing material comprises octadecyl silane, the octane bonded silica gel, the dodecyl bonded silica gel, this resin of polystyrene copolymerization divinyl.
17. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 3, it is characterized in that: the acid or neutral organic substance in described analyzing and testing meat and the aquatic products, the employed sorbing material that removes deproteinize, polypeptide, amino acid and fat, described sorbing material can be to have acid and lipophilic any or several compound substance simultaneously, or the potpourri of acid sorbing material and lipophilicity sorbing material.
18. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 18, it is characterized in that: described have acid and lipophilic any or several compound substance simultaneously, this material can be superpolymer or its finishing thing, or the bonded silica gel material, comprise various sulfonated polystyrene copolymerization divinylbenzene resins, carboxylic polystyrene copolymerization divinylbenzene resin; The high polymer material that contains sulfonic group, carboxyl or any one or several acid organo-functional group; The bonded silica gel material that contains sulfonic group, carboxyl or any one or several acid organo-functional group.
19. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 14, it is characterized in that: the potpourri of described acid sorbing material and lipophilicity sorbing material, this mixture material can be superpolymer or its finishing thing, or bonded silica gel material, the lipophilicity sorbing material that can be used as in the potpourri of acid sorbing material and lipophilicity sorbing material comprises octadecyl silane, the octane bonded silica gel, the dodecyl bonded silica gel, this resin of polystyrene copolymerization divinyl.
20. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 1, it is characterized in that: described utilization can remove deproteinize, polypeptide, the sorbing material of amino acid and fat optionally adsorbs from filtrate except that deproteinize, polypeptide, amino acid and fatty material, described to protein, polypeptide, the mode that the absorption of amino acid and fat can be adopted is included in disperses in the filtrate to add to remove deproteinize, polypeptide, amino acid can remove deproteinize with the sorbing material of fat or with filtrate by containing, polypeptide, the sorbing material of amino acid and fat.
21. the sample treatment that is used for detecting meat products and aquatic products objectionable impurities according to claim 20, it is characterized in that: described filtrate is by containing the sorbing material that can remove deproteinize, polypeptide, amino acid and fat, and the mode that can adopt comprises filtrate by being filled with the duckpin of sorbing material; With filtrate by being filled with the syringe filter of sorbing material; With filtrate by being filled with the liquid-transfering gun head of sorbing material; With filtrate by containing the filtering membrane of sorbing material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810182577A CN101750242A (en) | 2008-12-09 | 2008-12-09 | Sample pretreatment method for detecting harmful substances in meat product and aquatic product |
Applications Claiming Priority (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507945A (en) * | 2011-12-05 | 2012-06-20 | 河北省科学院生物研究所 | Sulfamethazine enzyme-linked immunoassay kit |
| CN109342149A (en) * | 2018-12-12 | 2019-02-15 | 江苏经贸职业技术学院 | A kind of harmful toxic matter detection device for fresh meat |
| CN110927280A (en) * | 2019-12-09 | 2020-03-27 | 江西科技师范大学 | Method for detecting harmful substances in aquatic products in green and high-sensitivity manner |
-
2008
- 2008-12-09 CN CN200810182577A patent/CN101750242A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507945A (en) * | 2011-12-05 | 2012-06-20 | 河北省科学院生物研究所 | Sulfamethazine enzyme-linked immunoassay kit |
| CN109342149A (en) * | 2018-12-12 | 2019-02-15 | 江苏经贸职业技术学院 | A kind of harmful toxic matter detection device for fresh meat |
| CN110927280A (en) * | 2019-12-09 | 2020-03-27 | 江西科技师范大学 | Method for detecting harmful substances in aquatic products in green and high-sensitivity manner |
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