CN109839466A - A method of testing melamine content in milk powder is detected based on three-dimensional magnetic molecularly imprinted polymer - Google Patents
A method of testing melamine content in milk powder is detected based on three-dimensional magnetic molecularly imprinted polymer Download PDFInfo
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Abstract
The invention belongs to technical field of food detection more particularly to a kind of methods based on three-dimensional magnetic molecularly imprinted polymer detection testing melamine content in milk powder.The invention firstly uses nitric acid-eutectic solvents to activate to multi-walled carbon nanotube；Then the multi-walled carbon nanotube of activation, graphene oxide etc. are mixed with to obtain three-dimensional magnetic solid phase extraction material using organic and inorganic reaction；Finally the melamine in powdered milk sample is extracted and detected using three-dimensional magnetic solid phase extraction material.Method extraction time of the invention is short, and extraction efficiency is high, can be suitble to the detection of melamine in a variety of milk powder and powder food product containing milk with a variety of Instrument crosslinkings such as high performance liquid chromatography, Capillary Electrophoresis, liquid chromatography-mass spectrography.
Description
Technical field
The invention belongs to technical field of food detection, more particularly to a kind of three-dimensional magnetic molecularly imprinted polymer that is based on to detect
The method of testing melamine content in milk powder.
Background technique
With people's level of consumption and improvement of living standard, consumer proposes higher want to the safety of food
It asks.Dairy products are a kind of indispensable food of people as daily nutrition substance.Currently, to the quality evaluation of dairy products be with
Protein content is index, mostly indicates the content of protein using the content of nitrogen at present.In order to improve crude protein content to reach
To the experimental standard of measurement nitrogen content, melamine is added to dairy products by some illegal businessmans
In.
The molecular formula of melamine is C3H6N6, is commonly called as melamine, extract of protein, and scientific name is " 2,4,6- tri- ammonia -1,3,5- tri-
Piperazine " is a kind of triazines nitrogen heterocyclic ring organic compound.Melamine is a kind of industrial chemicals, almost tasteless, and human body is arrived in intake
Interior to generate cyanuric acid, cyanuric acid and melamine can form big reticular structure, cause calculus, cause to kidney and bladder
Serious harm.Therefore the melamine in detection dairy produce has great importance to the safety for guaranteeing dairy produce.
Since dairy sample melamine concentration is low, and there are a large amount of protein, and matrix is complicated, cannot be directly used to examine
It surveys.Therefore the detection sensitivity for needing to use sample-pretreating method appropriate to improve melamine reduces matrix interference.Mesh
Before, have built up pre-treatment of a variety of methods for melamine in dairy produce, such as liquid-phase extraction, Solid Phase Extraction etc., but liquid
Mutually extraction can consume a large amount of organic solvent, and solid phase extraction manipulations are cumbersome and extraction efficiency is low.Therefore, the sample being simple and efficient is developed
Product pre-treating method has great importance for the melamine in rapid sensitive detection dairy produce.
Summary of the invention
When in order to solve the detection of dairy sample melamine, traditional sample-pretreating method organic solvent consumption is big, extracts
The problems such as taking low efficiency, the present invention provides one kind to be contained based on melamine in three-dimensional magnetic molecularly imprinted polymer detection milk powder
The method of amount.The present invention extracts melamine using the strong magnetic molecularly imprinted polymer of selectivity, improves extraction effect
The step of centrifugation is in turn avoided while rate and sensitivity realizes the rapid sensitive detection to melamine.
In order to achieve the above-mentioned object of the invention, the invention provides the following technical scheme:
A method of testing melamine content in milk powder being detected based on three-dimensional magnetic molecularly imprinted polymer, which is characterized in that packet
Include following steps:
(1) 4-6 g carbon nanotube the activation of carbon nanotube: is dispersed in 80-120 mL nitric acid-eutectic solvent mixed liquor
In, 4-6 h is stirred under the conditions of 80-90 DEG C, 600-800 rpm, to dispersion liquid cooled and filtered, obtained solid is washed with water
To neutrality, solid is dried in vacuo 12-14 h under the conditions of 60-80 DEG C, obtains the carbon nanotube of activation；
(2) preparation of three-dimensional magnetic compound: the nano graphene oxide of 2-3 g, 1-2 the g carbon nanotube activated are uniformly divided
It is dispersed in 250-400 mL deionized water-eutectic solvent mixed liquor, 1.5-2.0 g FeCl is added into dispersion liquid3·6H2O
It is uniformly mixed under 600-800 rpm mechanical stirring with 4.5-6 g NaAC, the polyethylene glycol mixing that 1.75-2.0 g is added is equal
It is even and be transferred in autoclave, under the conditions of 180-250 DEG C after pyroreaction 4-6 h, cold filtration, obtained solid
Ethyl alcohol, water washing 2-3 times are successively utilized, three-dimensional magnetic compound is dried to obtain；
(3) it the preparation of three-dimensional magnetic molecularly imprinted polymer: is scattered in after the three-dimensional magnetic compound that step (2) obtains is crushed
In deionized water-eutectic solvent mixed liquor, 0.05-0.1 g melamine, the mixing of 0.1-0.2 g acrylic acid are sequentially added
After uniformly, 0.2-0.4 g ethylene glycol dimethacrylate and 0.01-0.02 g azo isobutyronitrile is added, at 55-70 DEG C,
10-12h is reacted under 600-800 rpm mechanical stirring, material is adsorbed using magnet, the solid being adsorbed onto successively is used into water
With ethanol washing 3 times, through drying, crush three-dimensional magnetic molecularly imprinted polymer is prepared；
(4) preparation of powdered milk sample: taking 3-5 g milk powder and mixes it with 6-10 mL methanol-water mixture, at 45-60 DEG C,
It is centrifuged after ultrasound 15-25min under the conditions of 400-600 W, takes clear liquid up to powdered milk sample；
(5) extraction of melamine detects in powdered milk sample: the three-dimensional magnetic molecularly imprinted polymer of 4-5 mg is added to 8-
Ultrasound 1-2 min in 10 mL powdered milk samples mixes 3-5 min under 200-300 rpm revolving speed, is adsorbed using external magnet
Three-dimensional magnetic molecularly imprinted polymer simultaneously outwells supernatant, using 100 μ L ammonium hydroxide -1 min of methyl alcohol mixed liquor ultrasound to three
Dimension magnetic molecularly imprinted polymer is eluted, then by finally utilizing efficient liquid phase after magnet adsorbing separation imprinted polymer
Chromatography analyzes the melamine in supernatant.
Preferably, the diameter of carbon nanotube as described in step (1) is 5-10 nm；In the nitric acid-eutectic solvent
Eutectic solvent is choline chloride-glycerol, choline chloride-ethylene glycol, tetramethyl chlorination nitrogen-glycerol, tetramethyl ammonium chloride-second two
One of alcohol, the concentration of the eutectic solvent are 0.4-0.6 g/mL, and the concentration of the nitric acid is 1-2mol/L.
Preferably, the partial size of nano graphene oxide described in step (2) is 20-40 nm;The eutectic is molten
Agent is eutectic solvent used in step (1), the volume point of eutectic solvent in the deionized water-eutectic solvent mixed liquor
Number is 5-15 %；Concentration of the three-dimensional magnetic composite powder in deionized water-eutectic solvent mixed liquor is 0.2-
0.04 g /mL。
Preferably, eutectic solvent described in step (3) is choline chloride-acrylic acid, choline chloride-itaconic acid, four
One of ammonio methacrylate-acrylic acid, tetramethyl ammonium chloride-itaconic acid；The deionized water-eutectic solvent mixed liquor
The concentration of middle eutectic solvent is 0.02-0.1 g/mL;The three-dimensional magnetic compound is mixed in deionized water-eutectic solvent
Concentration in conjunction is 0.02-0.05 g/mL.
Preferably, the partial size of three-dimensional magnetic molecularly imprinted polymer described in step (3) is not more than 100 nm.
Preferably, the volume fraction of methanol is 15-25 % in methanol-water mixture described in step (4)；The first
Contain 0.01 g/mL NaCl in alcohol-water mixtures.
Preferably, the volume fraction of methanol is 35-50 % in ammonium hydroxide-methyl alcohol mixed liquor described in step (5).
The method of the present invention matrix interference is small, high sensitivity, compared with prior art, of the present invention a kind of based on three-dimensional
The method of magnetic molecularly imprinted polymer detection testing melamine content in milk powder has the advantages that the present invention using special
Property molecular engram material selective extraction is carried out to melamine, method extraction efficiency is high, matrix effect is small；Magnetic material is transferred
The step of being connected in molecularly imprinted polymer, being centrifuged when reducing extraction, shortens extraction time；Using eutectic solvent as
The solvent and dressing agent of reaction, not only reduce the consumption of organic solvent and eutectic reagent can be used as functional polymerization
Object, the adsorption effect of reinforcement material.The present invention can be with a variety of instrument such as high performance liquid chromatography, Capillary Electrophoresis, liquid chromatography-mass spectrography
Device combination, is suitble to the detection of melamine in a variety of milk powder and powder food product containing milk.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but embodiment is not to the technology of the present invention side
The restriction of case, it is all based on variation made by the present invention or equivalent replacement, it is within the scope of protection of the invention.
Embodiment one
A method of testing melamine content in milk powder being detected based on three-dimensional magnetic molecularly imprinted polymer, which is characterized in that packet
Include following steps:
(1) 5 g carbon nanotubes the activation of carbon nanotube: are dispersed in -0.45 g/mL chlorination gallbladder of 100 mL 2mol/L nitric acid
In alkali-glycerol eutectic solvent mixed liquor, 5 h are stirred under the conditions of 90 DEG C, 700 rpm, to dispersion liquid cooled and filtered,
After obtained solid is washed with water to neutrality, 13 h will be dried in vacuo under the conditions of 70 DEG C of solid, obtains the carbon nanotube of activation；
(2) preparation of three-dimensional magnetic compound: 2.5 g nano graphene oxides, 1 the g carbon nanotube activated are dispersed in
In 300 mL deionized water -10 % (v/v) choline chloride-glycerol eutectic solvent mixed liquor, 1.5 g are added into dispersion liquid
FeCl3·6H2O and 4.5 g NaAC is uniformly mixed under 700 rpm mechanical stirrings, and 1. 5 g polyethylene glycol are added and are uniformly mixed
And be transferred in autoclave, under the conditions of 220 DEG C after 4 h of pyroreaction, cold filtration, obtained solid is successively utilized
Ethyl alcohol, water washing 2 times, are dried to obtain three-dimensional magnetic compound；
(3) preparation of three-dimensional magnetic molecularly imprinted polymer: step (2) is obtained being scattered in after three-dimensional magnetic compound crushes
In -0.15 g/mL choline chloride of ionized water-acrylic acid eutectic solvent mixed liquor, sequentially add 0.06 g melamine,
0.15g acrylic acid is uniformly mixed, and 0.3 g ethylene glycol dimethacrylate and 0.01g azo isobutyronitrile is added, at 60 DEG C,
Material is adsorbed using magnet after reacting 11h under 700 rpm mechanical stirrings, the solid being adsorbed onto successively is used into water and ethyl alcohol
Three-dimensional magnetic molecularly imprinted polymer is prepared through drying, crushing in washing 3 times；
(4) preparation of powdered milk sample: taking 4 g milk powder and mixes it with -0.01 g/mL NaCl water mixed liquid of 8 mL, 15 % methanol
It 25 min of ultrasound and is centrifuged under the conditions of 50 DEG C, 500 W after conjunction, takes clear liquid up to powdered milk sample；
(5) extraction of melamine detects in powdered milk sample: 4 mg three-dimensional magnetic molecularly imprinted polymers are added to 8 mL milk
1 min of ultrasound, mixes 4 min under 250 rpm revolving speeds in powder sample, is printed using external magnet absorption three-dimensional magnetic molecule
Mark polymer simultaneously outwells supernatant, using 100 μ L ammonium hydroxide -45% methyl alcohol mixed liquor ultrasound, 1 min to three-dimensional magnetic molecule
Imprinted polymer is eluted, then by magnet adsorbing separation imprinted polymer, finally using high performance liquid chromatography to supernatant
In melamine analyzed.
Embodiment two
A method of testing melamine content in milk powder being detected based on three-dimensional magnetic molecularly imprinted polymer, which is characterized in that packet
Include following steps:
(1) 6 g carbon nanotubes the activation of carbon nanotube: are dispersed in -0.45 g/mL chlorination gallbladder of 120 mL 2mol/L nitric acid
In alkali-ethylene glycol eutectic solvent mixed liquor, 5 h are stirred under the conditions of 90 DEG C, 800 rpm, the mistake after dispersion liquid is cooling
Filter, after obtained solid is washed with water to neutrality, is dried in vacuo 14 h under the conditions of 70 DEG C for solid, obtains the carbon nanometer of activation
Pipe；
(2) preparation of three-dimensional magnetic compound: the carbon nanotube that the nano graphene oxide of 3 g, 1.2 g are activated is evenly dispersed
In 350 mL deionized water -10% (v/v) choline chlorides-ethylene glycol eutectic solvent mixed liquor, 2.0 are added into dispersion liquid
g FeCl3·6H2O and 5.5 g NaAC is uniformly mixed under 700 rpm mechanical stirrings, and it is equal that the mixing of 1.5 g polyethylene glycol is added
Even and be transferred in autoclave, under the conditions of 250 DEG C after 4 h of pyroreaction, cold filtration, obtained solid is successively sharp
With ethyl alcohol, water washing 3 times, it is dried to obtain three-dimensional magnetic compound；
(3) preparation of three-dimensional magnetic molecularly imprinted polymer: step (2) is obtained being scattered in after three-dimensional magnetic compound crushes
In ionized water -0.15g/mL choline chloride-itaconic acid eutectic solvent mixed liquor, sequentially add 0.06 g melamine,
After mixing, 0.3 g ethylene glycol dimethacrylate and 0.01g azo isobutyronitrile is added, 60 in 0.15g acrylic acid
DEG C, material is adsorbed using magnet after 12 h are reacted under 700 rpm mechanical stirrings, by the solid being adsorbed onto successively use water and
Ethanol washing 3 times, three-dimensional magnetic molecularly imprinted polymer is prepared through drying, crushing；
(4) preparation of powdered milk sample: taking 4 g milk powder and mixes it with -0.01 g/mL NaCl water mixed liquid of 8 mL, 15 % methanol
It 25 min of ultrasound and is centrifuged under the conditions of 50 DEG C, 500 W after conjunction, takes clear liquid up to powdered milk sample；
(5) extraction of melamine detects in powdered milk sample: 5 mg three-dimensional magnetic molecularly imprinted polymers are added to 10 mL milk
In powder sample after 1 min of ultrasound, 4 min are mixed under 250 rpm revolving speeds, adsorb three-dimensional magnetic molecule using external magnet
Imprinted polymer simultaneously outwells supernatant, using -45 1 min of % methyl alcohol mixed liquor ultrasound of 100 μ L ammonium hydroxide to three-dimensional magnetic
Molecularly imprinted polymer is eluted, then by finally utilizing high performance liquid chromatography pair after magnet adsorbing separation imprinted polymer
Melamine in supernatant is analyzed.
Comparative example one
A method of testing melamine content in milk powder being detected based on three-dimensional magnetic molecularly imprinted polymer, which is characterized in that packet
Include following steps:
(1) activation of carbon nanotube: 6 g carbon nanotubes are dispersed in 120 mL, 2 mol/L nitric acid-water mixed liquid, 90
DEG C, 5 h are stirred under the conditions of 800 rpm, to dispersion liquid cooled and filtered, after obtained solid is washed with water to neutrality, by solid
14 h are dried in vacuo under the conditions of 70 DEG C, obtain the carbon nanotube of activation；
(2) preparation of three-dimensional magnetic compound: 3 g nano graphene oxides, 1.2 the g carbon nanotube activated are dispersed in
In 350 mL deionized water -10 % (v/v) methyl alcohol mixed liquor, 2.0 g FeCl are added into dispersion liquid3·6H2O and 5.5 g
NaAC after mixing, is added 1.5 g polyethylene glycol and is uniformly mixed and is transferred to autoclave under 700 rpm mechanical stirrings
In, 4 h of pyroreaction under the conditions of 250 DEG C, cold filtration, obtained solid successively utilizes ethyl alcohol, water washing 3 times, dry
To three-dimensional magnetic compound；
(3) preparation of three-dimensional magnetic molecularly imprinted polymer: step (2) is obtained being scattered in after three-dimensional magnetic compound crushes
In the ethyl alcohol of -40 % of ionized water, 0.06 g melamine, 0.15g acrylic acid are sequentially added after mixing, 0.3 g is added
Ethylene glycol dimethacrylate and 0.01g azo isobutyronitrile react 12 h and are utilized under 60 DEG C, 700 rpm mechanical stirrings
Magnet adsorbs material, and the solid being adsorbed onto successively is used water and ethanol washing 3 times, is prepared three through drying, crushing
Tie up magnetic molecularly imprinted polymer；
(4) preparation of powdered milk sample: taking 4 g milk powder and mixes it with -0.01 g/mL NaCl water mixed liquid of 8 mL, 15 % methanol
It 25 min of ultrasound and is centrifuged under the conditions of 50 DEG C, 500 W after conjunction, takes clear liquid up to powdered milk sample；
(5) extraction of melamine detects in powdered milk sample: the three-dimensional magnetic molecularly imprinted polymer of 5 mg is added to 10 mL
In powdered milk sample after 1 min of ultrasound, 4 min are mixed under 250 rpm revolving speeds, utilize external magnet absorption three-dimensional magnetic point
Sub- imprinted polymer simultaneously outwells supernatant, using 100 uL ammonium hydroxide -45% methyl alcohol mixed liquor ultrasound, 1 min to three-dimensional magnetic
Molecularly imprinted polymer is eluted, after then utilizing magnet adsorbing separation imprinted polymer, using high performance liquid chromatography to upper
Melamine in clear liquid is analyzed.
Comparative example two
In national standard GB/T22388-2008 in milk powder melamine pre-treatment detection method
(1) 2 g milk powder is taken to mix with 15 mL trichloroacetic acids and 5 mL acetonitriles, 10 min of ultrasound, then vibrate after 10 min
It is centrifuged 5 min under the conditions of 5000 rpm/min, obtains supernatant, clear liquid is filtered, obtains powdered milk sample；
(2) powdered milk sample is transferred to solid-phase extraction column, is successively washed, is drained with 3 mL water and 3 mL methanol, with 6 mL's
Eluent is collected in the elution of amination methanol, and the flow velocity of sample is 0.8 mL/min, and nitrogen is blown under the conditions of 50 DEG C by eluent
It is dry, after residue flows phased soln with 1 mL, analyzed using high performance liquid chromatography.
Method Performance
(1) quantitative limit is used as using 3 times of instrument signal/noise ratio as detection limit and 10 times of signal-to-noise ratio, detection embodiment 1,2 and right
The sensitivity of ratio 1,2 methods.
(2) with the extraction efficiency of following formula calculation method, embodiment 1,2 and comparative example 1, the extraction effect of 2 methods are detected
Fruit.
V in formula, c analyze the volume of sample and the concentration of melamine before respectively indicating sample introduction, and m indicates melamine in sample
The quality of amine.
The comparison of the analysis parameter of method in embodiment 1,2 and comparative example 1,2
As can be seen from the table, the three-dimensional magnetic molecularly imprinted polymer prepared compared to traditional solvent, what the present invention used
The three-dimensional magnetic molecularly imprinted polymer of eutectic solvent preparation is higher to the sensitivity of melamine；It is solid compared to common
Phase extracting process, extraction time of the invention is short, and extraction efficiency is high, high sensitivity, has broader practice prospect.
Claims (7)
1. a kind of method based on three-dimensional magnetic molecularly imprinted polymer detection testing melamine content in milk powder, which is characterized in that
The following steps are included:
(1) 4-6 g carbon nanotube the activation of carbon nanotube: is dispersed in 80-120 mL nitric acid-eutectic solvent mixed liquor
In, 4-6 h is stirred under the conditions of 80-90 DEG C, 600-800 rpm, to dispersion liquid cooled and filtered, obtained solid is washed with water
To neutrality, solid is dried in vacuo 12-14 h under the conditions of 60-80 DEG C, obtains the carbon nanotube of activation；
(2) preparation of three-dimensional magnetic compound: the nano graphene oxide of 2-3 g, 1-2 the g carbon nanotube activated are uniformly divided
It is dispersed in 250-400 mL deionized water-eutectic solvent mixed liquor, 1.5-2.0 g FeCl is added into dispersion liquid3·6H2O
It is uniformly mixed under 600-800 rpm mechanical stirring with 4.5-6 g NaAC, the polyethylene glycol mixing that 1.75-2.0 g is added is equal
It is even and be transferred in autoclave, under the conditions of 180-250 DEG C after pyroreaction 4-6 h, cold filtration, obtained solid
Ethyl alcohol, water washing 2-3 times are successively utilized, three-dimensional magnetic compound is dried to obtain；
(3) it the preparation of three-dimensional magnetic molecularly imprinted polymer: is scattered in after the three-dimensional magnetic compound that step (2) obtains is crushed
In deionized water-eutectic solvent mixed liquor, 0.05-0.1 g melamine, the mixing of 0.1-0.2 g acrylic acid are sequentially added
After uniformly, 0.2-0.4 g ethylene glycol dimethacrylate and 0.01-0.02 g azo isobutyronitrile is added, at 55-70 DEG C,
10-12h is reacted under 600-800 rpm mechanical stirring, material is adsorbed using magnet, the solid being adsorbed onto successively is used into water
With ethanol washing 3 times, through drying, crush three-dimensional magnetic molecularly imprinted polymer is prepared；
(4) preparation of powdered milk sample: taking 3-5 g milk powder and mixes it with 6-10 mL methanol-water mixture, at 45-60 DEG C,
It is centrifuged after ultrasound 15-25min under the conditions of 400-600 W, takes clear liquid up to powdered milk sample；
(5) extraction of melamine detects in powdered milk sample: the three-dimensional magnetic molecularly imprinted polymer of 4-5 mg is added to 8-
Ultrasound 1-2 min in 10 mL powdered milk samples mixes 3-5 min under 200-300 rpm revolving speed, is adsorbed using external magnet
Three-dimensional magnetic molecularly imprinted polymer simultaneously outwells supernatant, using 100 μ L ammonium hydroxide -1 min of methyl alcohol mixed liquor ultrasound to three
Dimension magnetic molecularly imprinted polymer is eluted, then by finally utilizing efficient liquid phase after magnet adsorbing separation imprinted polymer
Chromatography analyzes the melamine in supernatant.
2. according to claim 1 a kind of based on three-dimensional magnetic molecularly imprinted polymer detection testing melamine content in milk powder
Method, which is characterized in that the diameter of carbon nanotube as described in step (1) be 5-10 nm；Nitric acid-the eutectic is molten
Eutectic solvent is choline chloride-glycerol, choline chloride-ethylene glycol, tetramethyl chlorination nitrogen-glycerol, tetramethyl ammonium chloride-in agent
One of ethylene glycol, the concentration of the eutectic solvent are 0.4-0.6 g/mL, and the concentration of the nitric acid is 1-2 mol/L.
3. one kind according to claim 1 is contained based on melamine in three-dimensional magnetic molecularly imprinted polymer detection milk powder
The method of amount, which is characterized in that the partial size of nano graphene oxide described in step (2) is 20-40 nm;Described is low total
Molten solvent is eutectic solvent used in step (1), the body of eutectic solvent in the deionized water-eutectic solvent mixed liquor
Fraction is 5-15 %；Concentration of the three-dimensional magnetic composite powder in deionized water-eutectic solvent mixed liquor is
0.2-0.04 g /mL。
4. one kind according to claim 1 is contained based on melamine in three-dimensional magnetic molecularly imprinted polymer detection milk powder
The method of amount, which is characterized in that eutectic solvent described in step (3) is choline chloride-acrylic acid, choline chloride-clothing health
One of acid, tetramethyl ammonium chloride-acrylic acid, tetramethyl ammonium chloride-itaconic acid；Deionized water-the eutectic solvent
The concentration of eutectic solvent is 0.02-0.1 g/mL in mixed liquor;The three-dimensional magnetic compound is in deionized water-eutectic
Concentration in solvent mixing is 0.02-0.05 g/mL.
5. one kind according to claim 1 is contained based on melamine in three-dimensional magnetic molecularly imprinted polymer detection milk powder
The method of amount, which is characterized in that the partial size of three-dimensional magnetic molecularly imprinted polymer described in step (3) is not more than 100 nm.
6. one kind according to claim 1 is contained based on melamine in three-dimensional magnetic molecularly imprinted polymer detection milk powder
The method of amount, which is characterized in that the volume fraction of methanol is 15-25 % in methanol-water mixture described in step (4)；Institute
Contain 0.01 g/mL NaCl in the methanol-water mixture stated.
7. one kind according to claim 1 is contained based on melamine in three-dimensional magnetic molecularly imprinted polymer detection milk powder
The method of amount, which is characterized in that the volume fraction of methanol is 35-50 in ammonium hydroxide-methyl alcohol mixed liquor described in step (5)
%。
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| CN113740461A (en) * | 2021-09-08 | 2021-12-03 | 河北北方学院 | Method for detecting pesticide residue of eutectic solvent magnetic carbon nanotube dispersed solid phase extraction bactericide |
| CN114324658A (en) * | 2021-12-30 | 2022-04-12 | 福州大学 | Dispersive solid-phase extraction-high performance liquid chromatography combined detection method for melamine |
| CN117310050A (en) * | 2023-11-28 | 2023-12-29 | 中国中医科学院中医药健康产业研究所 | Screening method of honeysuckle antioxidation quality markers |
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| CN113740461A (en) * | 2021-09-08 | 2021-12-03 | 河北北方学院 | Method for detecting pesticide residue of eutectic solvent magnetic carbon nanotube dispersed solid phase extraction bactericide |
| CN113740461B (en) * | 2021-09-08 | 2024-04-09 | 河北北方学院 | Method for detecting pesticide residues of eutectic solvent magnetic carbon nanotube dispersed solid phase extraction bactericide |
| CN114324658A (en) * | 2021-12-30 | 2022-04-12 | 福州大学 | Dispersive solid-phase extraction-high performance liquid chromatography combined detection method for melamine |
| CN114324658B (en) * | 2021-12-30 | 2023-11-14 | 福州大学 | Method for detecting melamine by combining dispersion solid phase extraction and high performance liquid chromatography |
| CN117310050A (en) * | 2023-11-28 | 2023-12-29 | 中国中医科学院中医药健康产业研究所 | Screening method of honeysuckle antioxidation quality markers |
| CN117310050B (en) * | 2023-11-28 | 2024-02-09 | 中国中医科学院中医药健康产业研究所 | Screening method of honeysuckle antioxidation quality markers |
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