CN106990183A - The method for chromatographic determination of synthetic coloring matter in a kind of food - Google Patents
The method for chromatographic determination of synthetic coloring matter in a kind of food Download PDFInfo
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- CN106990183A CN106990183A CN201710310734.3A CN201710310734A CN106990183A CN 106990183 A CN106990183 A CN 106990183A CN 201710310734 A CN201710310734 A CN 201710310734A CN 106990183 A CN106990183 A CN 106990183A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention disclose the method for chromatographic determination of synthetic coloring matter in food a kind of, including step sample extraction, sample purification, configuration artificial tanning agent's hybrid standard application liquid, by artificial tanning agent's hybrid standard application liquid injection hplc determination, Detection wavelength:Lemon yellow 428mm, amaranth 521mm, indigo carmine 608mm, carmine 509 mm, the mm of sunset yellow 483, red 507 mm of temptation, the mm of light blue 625 and the mm of erythrosine 529;The liquid chromatogram and peak area of eight kinds of artificial synthesized colouring agents are obtained, the linear equation of standard series is drawn;Sample solution is injected into hplc determination, sample chromatogram peak is obtained, retention time is qualitative;Sample peak area brings the linear equation of standard series into, calculates the concentration of target compound, quantified by external standard method;According to formulaCalculate the content of eight kinds of artificial synthesized colouring agents;This method is fast and convenient, sensitivity is high, disturb less, result is accurate, favorable reproducibility, can preferably be applied to the detection of actual food product sample.
Description
Technical field
The present invention relates to synthetic coloring matter detection technique field, the chromatographic determination of synthetic coloring matter in specifically a kind of food
Method.
Background technology
The U.S.A for pursuing outward appearance is the nature of people, and people are also required to dress up to the food eaten.Candy, the tempting egg of the five colours
Cake, scarlet sugarcoated haws, there's no one who doesn't or isn't allow people to drool with envy.All these in riotous profusion colorful colors all be unable to do without pigment in fact.Naturally
Food easily fades or changed colour during processing is preserved, so people often add pigment during processed food.
Pigment can be divided into natural pigment and artificial color, and natural pigment is mainly extracted in plant tissue, also including coming
From the pigment of animal and microorganism, unstability and expensive, the food industry artificial conjunction of use mostly due to natural pigment
Into pigment.
The aniline dyes separated in the main oil using coking of synthetic dyestuff is made up of raw material, so being referred to as coking pigment
Or aniline dye, with lead to diarrhea, cause prominent property(Gene mutation), carcinogenesis, be used in GB2760 standards strict
Dosage limitation, therefore accurate quick detection synthetic dyestuff is even more important.
At present, the detection method of synthetic dyestuff is GB/T5009.35, though being revised by 2016, the standard has following lack
Fall into:First, adsorbed using Silon, it is big that trivial operations expend the artificial intensity of reagent;2nd, due to the sodium benzoate structure of erythrosine
It can not be adsorbed by Silon, therefore erythrosine and other pigments together extraction and cleaning, erythrosine can not be unable to Simultaneous Determination,
Need with upper machine testing again after liquid-liquid extraction;3rd, minimum detectability is 0.2~0.5mg/kg, and concentrations are high, and sensitivity is low;
4th, due to being adsorbed using Silon, sample will extraction and cleaning one by one, be not suitable for batch sample detection.5th, the standard method is not
Formulate the high-fat sample detection steps such as ham sausage, sausage stuffed mainly with bean starch paste, sausage.
The content of the invention
It is an object of the invention to provide a kind of method for chromatographic determination of synthetic coloring matter in food, this method can be from food
It is disposable in product to extract lemon yellow, amaranth, indigo carmine, famille rose, sunset yellow, the eight kinds of conjunctions of the red, light blue of temptation and erythrosine
Into colouring agent, carry out liquid chromatogram measuring synchronous high-efficiency.
The technical solution adopted for the present invention to solve the technical problems is:
The method for chromatographic determination of synthetic coloring matter, comprises the following steps in a kind of food:
S1, sample extraction
2g food samples are weighed into centrifuge tube, a)For liquid food sample, acetic acid zinc solution and potassium oxalate/phosphoric acid hydrogen are added
Two potassium solutions, precipitating proteins, then pH to 6 is adjusted with 10% ammoniacal liquor, 10 mL are then settled to water, centrifugal treating obtains treating net
The sample supernatant of change;b)For preparing drinks sample, heating removes ethanol, adjusts pH to 6 with ammonia spirit, then uses water constant volume
To 10 mL, centrifugal treating obtains sample supernatant to be clean;c)For solid food sample, use ammoniated methanol molten after homogeneous
Liquid repeats to extract to extracting liquid colourless, merges extract solution and is evaporated in 60 DEG C of water-baths, 10 mL is settled to water, centrifugal treating is obtained
Sample supernatant to be clean;d)For meat sample, petroleum ether degreasing after homogeneous, then repeated with ammoniated methanol solution to extract extremely
Extracting liquid colourless, merges extract solution and is evaporated in 60 DEG C of water-baths, 10 mL are settled to water, centrifugal treating obtains sample to be clean
Supernatant;
S2, sample purification
The sample supernatant for taking 5 mL steps S1 to obtain, with 1 mL/min speed by weak anionic solid-phase extraction column, then divides
Weak anionic solid-phase extraction column is not eluted with the 6 mL pH4 aqueous solution, the 6 mL pH6 aqueous solution and 6 mL methanol, then will be weak
Anion solid-phase extraction column is passed through air blow drying;Eluted and collected with 6 mL ammoniated methanols afterwards, 60 DEG C of water-bath nitrogen dryings, then
Plus 1 mL water redissolve, mix, supernatant is sample solution, feed flow analysis of hplc;
S3, configuration artificial tanning agent's hybrid standard application liquid
Accurately pipette appropriate 0.5 mg/mL lemon yellows standard reserving solution, 0.5 mg/mL amaranths standard reserving solution, 0.5 mg/mL
Carmine red standard storing solution, 0.5 mg/mL sunset yellows standard reserving solution, 1.0 mg/mL lure red standard reserving solution, 0.5 mg/
ML light blues standard reserving solution, 1.0 mg/mL erythrosines standard reserving solutions and 0.5 mg/mL indigo carmine standard reserving solutions, and
0.2 μ g/mL, 0.5 μ g/mL, 2.0 μ g/mL, 5.0 μ g/mL, 10 μ g/mL and 20 μ g/mL serial people are configured to water
Work colouring agent hybrid standard application liquid;
S4, the artificial tanning agent's hybrid standard application liquid for configuring step S3 inject hplc determination, liquid chromatogram measuring
Condition is:Chromatographic column:C18,4.6 × 250 mm, 5 μm;Mobile phase:A is ammonium acetate solution, and B is methanol;Flow velocity:1.0
mL/min;Column temperature:30℃;Sample size:20 µL;Gradient elution program:0.0~5.0min, 80%A~65%A and 20~35%B;
5.0~12.0min, 65%A~20%A and 35~80%B;12.0~16.0min, 20%A and 80%B;16.0~17.0min,
20%A~80%A and 80~20%B;17.0~20.0min, 80%A and 20%B;Detection wavelength:Lemon yellow 428mm, amaranth
521mm, indigo carmine 608mm, carmine 509 mm, the mm of sunset yellow 483, red 507 mm of temptation, the mm of light blue 625 and red moss
Red 529 mm;The liquid chromatogram and peak area of eight kinds of artificial synthesized colouring agents are obtained, the linear equation of standard series is drawn;
S5, the sample solution for obtaining step S2 inject hplc determination, and liquid chromatogram measuring condition is identical with step S3,
Sample chromatogram peak is obtained, retention time is qualitative;Sample peak area brings the linear equation of standard series into, calculates target compound
Concentration, quantified by external standard method;
S6, according to formulaCalculate the content of eight kinds of artificial synthesized colouring agents;X tries for sample in above formula
Target compound content in sample, C is target compound content, V in the sample specimens solution obtained by the linear equation of standard
For the final constant volume of sample specimens, m is the quality of sample specimens, and f is sample specimens extension rate;With repeated bar
The arithmetic mean of instantaneous value of the measurement result independent twice obtained under part is represented, as a result retains three effective digitals.
The beneficial effects of the invention are as follows:Weak anionic solid phase extraction column stuffing adsorbs red scarlet in neutral conditions, acid
Under the conditions of adsorb other synthetic coloring matters, the characteristic of all synthetic coloring matters of desorption, can disposably be carried in the basic conditions
8 kinds of artificial synthesized colouring agents of purification are taken, and apply Full-automatic solid phase extraction instrument, sample can be handled with automatic batch, expend examination
Agent is few, reduces manual labor amount;UV-detector, full wavelength scanner, every kind of pigment correspondence are replaced with PDAD
Optimal wavelength, minimum detectability reaches 0.025mg/kg, and remolding sensitivity original method is higher by 5~10 times;This method is fast and convenient, spirit
Sensitivity is high, disturb less, result is accurate, favorable reproducibility, can preferably be applied to the detection of actual food product sample.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples:
Fig. 1 is eight kinds of artificial synthesized colouring agent reference colour spectrograms of the invention.
Embodiment
The present invention provides a kind of method for chromatographic determination of synthetic coloring matter in food, it is adaptable to lemon yellow, three-coloured amaranth in food
Red, indigo carmine, famille rose, sunset yellow, eight kinds of synthetic coloring matter high performance liquid chromatography of the red, light blue of temptation and erythrosine are determined;
Lemon yellow, amaranth, indigo carmine, famille rose, sunset yellow, the detection limit for luring red, light blue and erythrosine in this method
For:0.025 mg/kg, is quantitatively limited to:0.075 mg/kg.
In order to more easily describe the present invention, first reagent used in the present invention is listed herein, in addition to especially indicating,
The present embodiment agents useful for same is that analysis is pure, and water is to meet one-level water as defined in GB/T 6682;
3.1 methanol(CH3OH):Chromatographically pure;
3.2 ammoniacal liquor(NH3•H2O);
3.3 citric acid(C6H8O7•H2O);
3.4 zinc acetate(C4H6O4Zn•2H2O);
3.5 ammonium acetate(CH3COONH4):Top pure grade;
3.6 potassium oxalate(C2O4K2•H2O);
3.7 dipotassium hydrogen phosphate(K2HPO4);
3.8 petroleum ether(30 DEG C~60 DEG C);
3.9 acetic acid zinc solution(1.0 mol/L):Weigh 22 g zinc acetates(3.4), dissolved with water and be settled to 100 mL, mixed
It is even;
3.10 potassium oxalates/dipotassium hydrogen phosphate solution:Weigh 3.0 g potassium oxalates(3.6)With 7.0 g dipotassium hydrogen phosphates(3.7), use
Water dissolves and is settled to 100 mL, mixes;
3.11 citric acid solution:Weigh 20g citric acids(3.3), dissolved with water and be settled to 100 mL, mixed;
3.12 ammonia spirit(10%):Take 10 mL ammoniacal liquor(3.2), 100 mL are settled to water, are mixed;
3.13 the pH4 aqueous solution:Water adding citric acid solution(3.11)PH value is adjusted to 4;
3.14 the pH6 aqueous solution:Water adding citric acid solution(3.11)PH value is adjusted to 6;
3.15 ammoniated methanol solution(3%):Take 3 mL ammoniacal liquor(3.2)It is added to 97 mL methanol(3.1)In, mix;
3.16 ammonium acetate solution(0.02 mol/L):Weigh 1.54 g ammonium acetates(3.5), dissolved with water and be settled to 1000
ML, is mixed, and crosses 0.45 μm of filter membrane;
3.17 standard items:Lemon yellow standard reserving solution(0.5 mg/mL), amaranth standard reserving solution(0.5 mg/mL), kermes
Red standard reserving solution(0.5 mg/mL), sunset yellow standard reserving solution(0.5 mg/mL), lure red standard reserving solution(1.0 mg/
mL), light blue standard reserving solution(0.5 mg/mL)With erythrosine standard reserving solution(1.0 mg/mL)(Ground purchased from Chinese measuring science
Study carefully institute), indigo carmine solid etalon product(Purity >=99.9%, purchased from Dr. Ehrenstorfer companies);
3.18 standard liquid is configured:
3.18.1 indigo carmine standard reserving solution(0.5 mg/mL):Accurately weigh appropriate indigo carmine solid etalon product
(3.17), with water dissolving and constant volume, mix;
3.18.2 hybrid standard application liquid(100 µg/mL):Appropriate synthetic coloring matter standard reserving solution is pipetted respectively(3.17 and
3.18.1), water constant volume is used, is mixed;
3.18.3 hybrid standard is serial:Accurately pipette appropriate hybrid standard application liquid(3.18.2), 0.2 μ g/ are configured to water
ML, 0.5 μ g/mL, 2.0 μ g/mL, 5.0 μ g/mL, 10 μ g/mL and 20 μ g/mL hybrid standard series.
With reference to shown in Fig. 1, the present invention specifically includes following steps:
S1, sample extraction
2g food samples are weighed into centrifuge tube, a)For liquid food sample, such as liquid beverage, liquid quelite and fruit juice
Deng, addition acetic acid zinc solution and potassium oxalate/dipotassium hydrogen phosphate solution, precipitating proteins, then adjust pH to 6, Ran Houyong with 10% ammoniacal liquor
Water is settled to 10 mL, and 4000 r/min centrifuge 10 min, obtain sample supernatant to be clean;
b)For preparing drinks sample, heating removes ethanol, adjusts pH to 6 with ammonia spirit, 10 mL are then settled to water,
4000 r/min centrifuge 10 min, obtain sample supernatant to be clean;
c)For solid food sample, such as preserved fruit, candy, jelly, tinned fruit, corn flour, millet, millet powder, homogeneous
Repeated to extract to extracting liquid colourless with ammoniated methanol solution afterwards, merge extract solution and evaporated in 60 DEG C of water-baths, 10 are settled to water
ML, 10000 r/min centrifuge 3 min, obtain sample supernatant to be clean;
d)For meat sample, such as ham sausage, sausage, sausage stuffed mainly with bean starch paste, petroleum ether degreasing after homogeneous, then with ammoniated methanol solution weight
It is multiple to extract to extracting liquid colourless, merge extract solution and evaporated in 60 DEG C of water-baths, 10 mL are settled to water, centrifugal treating obtains treating net
The sample supernatant of change;
S2, sample purification
The sample supernatant for taking 5 mL steps S1 to obtain, with 1 mL/min speed by weak anionic solid-phase extraction column, then divides
Weak anionic solid-phase extraction column is not eluted with the 6 mL pH4 aqueous solution, the 6 mL pH6 aqueous solution and 6 mL methanol, then will be weak
Anion solid-phase extraction column is passed through air blow drying;Eluted and collected with 6 mL ammoniated methanols afterwards, 60 DEG C of water-bath nitrogen dryings, then
Plus 1 mL water redissolve, mix, supernatant is sample solution, feed flow analysis of hplc;
S3, configuration artificial tanning agent's hybrid standard application liquid
Accurately weigh 0.5 mg/mL lemon yellows standard reserving solution, 0.5 mg/mL amaranths standard reserving solution, 0.5 mg/mL kermes
Red standard reserving solution, 0.5 mg/mL sunset yellows standard reserving solution, 1.0 mg/mL lure red standard reserving solution, 0.5 mg/mL bright
Blue standard reserving solution, 1.0 mg/mL erythrosines standard reserving solutions and 0.5 mg/mL indigo carmine standard reserving solutions, and use water
The series for being configured to 0.2 μ g/mL, 0.5 μ g/mL, 2.0 μ g/mL, 5.0 μ g/mL, 10 μ g/mL and 20 μ g/mL is artificial
Toner hybrid standard application liquid;
S4, the artificial tanning agent's hybrid standard application liquid for configuring step S3 inject hplc determination, liquid chromatogram measuring
Condition is:
Chromatographic column:C18,4.6 × 250 mm, 5 μm;
Mobile phase:A is ammonium acetate solution, and B is methanol;
Flow velocity:1.0 mL/min;Column temperature:30℃;
Sample size:20 µL;Detector:PDAD(PDA)Or UV-detector(TUV);
Gradient elution program:It is shown in Table 1
The gradient elution program of table 1
Eight kinds of synthetic coloring matter Detection wavelengths:It is shown in Table 2
2 eight kinds of synthetic coloring matter Detection wavelengths of table
The liquid chromatogram and peak area of eight kinds of artificial synthesized colouring agents are obtained, the linear equation of standard series is drawn;
S5, the sample solution for obtaining step S2 inject hplc determination, and liquid chromatogram measuring condition is identical with step S3,
Sample chromatogram peak is obtained, retention time is qualitative;Sample peak area brings the linear equation of standard series into, calculates target compound
Concentration, quantified by external standard method;
S6, according to formulaCalculate the content of eight kinds of artificial synthesized colouring agents;X is sample in above formula
Target compound content in sample, C is target compound content in the sample specimens solution obtained by the linear equation of standard,
V is the final constant volume of sample specimens, and m is the quality of sample specimens, and f is sample specimens extension rate;With repeatability
Under the conditions of the arithmetic mean of instantaneous value of measurement result independent twice that obtains represent, as a result retain three effective digitals.
In order to obtain more accurate measurement result, inspection reagent, experimental water used in the present invention etc. can be injected
Liquid chromatograph enters line blank test, if containing detection material, to be deducted in result of calculation, or reconfigure new examination
Agent and experimental water.
Most of synthetic coloring matters such as lemon yellow are benzene sulfonic acid sodium salt structure, can be adsorbed by Silon under acid condition, and
Erythrosine is sodium benzoate structure, and acid condition can not be adsorbed by Silon.This method uses weak anionic solid-phase extraction column,
Can determine simultaneously lemon yellow, amaranth, indigo carmine, famille rose, sunset yellow, lure the benzene sulfonic acid sodium salt structure such as red, light blue and
The synthetic coloring matter of the sodium benzoate structure such as erythrosine.
The filling-material structure of weak anionic solid-phase extraction column shows:When solution pKa is more than-NH2 two units of pKa, fill out
- NH2 in material just exists with the cationic state of ammonium ion, and now it can just adsorb what some existed with anionic state
Object;And when pKa is less than-NH2 two units of pKa, ammonium ion exists with-NH2 states, anion object will
Desorption, is eluted by certain solvent;Therefore, sample extracting solution pH is adjusted to 6 or so before loading, is to ensure weak anionic
The synthetic coloring matter of solid-phase extraction column P-TOLUENE SULFO ACID 99's sodium structure and sodium benzoate structure has suction-operated, finally uses ammoniated methanol
Solution(3%)Determinand is eluted out.
Drying pillar is to be dried up moisture, prevent that nitrogen blows overlong time below, and if excess moisture before elution
In the presence of, ammoniated methanol below can be diluted, making the concentration of methanol reduces, elution effect can be impacted.
To ensure the effect of loading, elution and elution in purification process, flow control is in no more than 1mL/min.
Because a variety of synthetic coloring matters can be reproduced the absorption of the water system such as cellulose filter membrane, therefore can not use membrane filtration sample
Product, if sample solution is muddy, can 4000 r/min centrifuge 10 min, machine is determined on supernatant.
When being detected with UV-detector, wavelength switching pattern may be selected, the maximum absorption band for making eight kinds of synthetic coloring matters is in
On a present collection of illustrative plates.
The above described is only a preferred embodiment of the present invention, not making any formal limitation to the present invention;Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible variations and modification to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, every content without departing from technical solution of the present invention, the technical spirit according to the present invention is done to above example
Any simple modification, equivalent substitution, equivalence changes and modification, still fall within technical solution of the present invention protection in the range of.
Claims (1)
1. the method for chromatographic determination of synthetic coloring matter in a kind of food, it is characterised in that comprise the following steps:
S1, sample extraction
2g food samples are weighed into centrifuge tube, a)For liquid food sample, acetic acid zinc solution and potassium oxalate/phosphoric acid hydrogen are added
Two potassium solutions, precipitating proteins, then pH to 6 is adjusted with 10% ammoniacal liquor, 10 mL are then settled to water, centrifugal treating obtains treating net
The sample supernatant of change;b)For preparing drinks sample, heating removes ethanol, adjusts pH to 6 with ammonia spirit, then uses water constant volume
To 10 mL, centrifugal treating obtains sample supernatant to be clean;c)For solid food sample, use ammoniated methanol molten after homogeneous
Liquid repeats to extract to extracting liquid colourless, merges extract solution and is evaporated in 60 DEG C of water-baths, 10 mL is settled to water, centrifugal treating is obtained
Sample supernatant to be clean;d)For meat sample, petroleum ether degreasing after homogeneous, then repeated with ammoniated methanol solution to extract extremely
Extracting liquid colourless, merges extract solution and is evaporated in 60 DEG C of water-baths, 10 mL are settled to water, centrifugal treating obtains sample to be clean
Supernatant;
S2, sample purification
The sample supernatant for taking 5 mL steps S1 to obtain, with 1 mL/min speed by weak anionic solid-phase extraction column, then divides
Weak anionic solid-phase extraction column is not eluted with the 6 mL pH4 aqueous solution, the 6 mL pH6 aqueous solution and 6 mL methanol, then will be weak
Anion solid-phase extraction column is passed through air blow drying;Eluted and collected with 6 mL ammoniated methanols afterwards, 60 DEG C of water-bath nitrogen dryings, then
Plus 1 mL water redissolve, mix, supernatant is sample solution, feed flow analysis of hplc;
S3, configuration artificial tanning agent's hybrid standard application liquid
Accurately weigh 0.5 mg/mL lemon yellows standard reserving solution, 0.5 mg/mL amaranths standard reserving solution, 0.5 mg/mL kermes
Red standard reserving solution, 0.5 mg/mL sunset yellows standard reserving solution, 1.0 mg/mL lure red standard reserving solution, 0.5 mg/mL bright
Blue standard reserving solution, 1.0 mg/mL erythrosines standard reserving solutions and 0.5 mg/mL indigo carmine standard reserving solutions, and use water
The series for being configured to 0.2 μ g/mL, 0.5 μ g/mL, 2.0 μ g/mL, 5.0 μ g/mL, 10 μ g/mL and 20 μ g/mL is artificial
Toner hybrid standard application liquid;
S4, the artificial tanning agent's hybrid standard application liquid for configuring step S3 inject hplc determination, liquid chromatogram measuring
Condition is:Chromatographic column:C18,4.6 × 250 mm, 5 μm;Mobile phase:A is ammonium acetate solution, and B is methanol;Flow velocity:1.0
mL/min;Column temperature:30℃;Sample size:20 µL;Gradient elution program:0.0~5.0min, 80%A~65%A and 20~35%B;
5.0~12.0min, 65%A~20%A and 35~80%B;12.0~16.0min, 20%A and 80%B;16.0~17.0min,
20%A~80%A and 80~20%B;17.0~20.0min, 80%A and 20%B;Detection wavelength:Lemon yellow 428mm, amaranth
521mm, indigo carmine 608mm, carmine 509 mm, the mm of sunset yellow 483, red 507 mm of temptation, the mm of light blue 625 and red moss
Red 529 mm;The liquid chromatogram and peak area of eight kinds of artificial synthesized colouring agents are obtained, the linear equation of standard series is drawn;
S5, the sample solution for obtaining step S2 inject hplc determination, and liquid chromatogram measuring condition is identical with step S3,
Sample chromatogram peak is obtained, retention time is qualitative;Sample peak area brings the linear equation of standard series into, calculates target compound
Concentration, quantified by external standard method;
S6, according to formulaCalculate the content of eight kinds of artificial synthesized colouring agents;X is in sample specimens in above formula
Target compound content, C is target compound content in the sample specimens solution obtained by the linear equation of standard, and V is sample
The final constant volume of product sample, m is the quality of sample specimens, and f is sample specimens extension rate;Under the conditions of repeatability
The arithmetic mean of instantaneous value of the measurement result independent twice obtained is represented, as a result retains three effective digitals.
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CN111965270A (en) * | 2020-07-07 | 2020-11-20 | 浙江省食品药品检验研究院 | Method for detecting 8 synthetic colorants in glutinous rice food |
CN112684047A (en) * | 2020-12-21 | 2021-04-20 | 贵州省产品质量检验检测院 | Method for simultaneously detecting multiple artificially synthesized colorants in preserved fruits |
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