CN110455952A - Azo and aromatic amine compounds quick screening method in a kind of food - Google Patents
Azo and aromatic amine compounds quick screening method in a kind of food Download PDFInfo
- Publication number
- CN110455952A CN110455952A CN201910775447.9A CN201910775447A CN110455952A CN 110455952 A CN110455952 A CN 110455952A CN 201910775447 A CN201910775447 A CN 201910775447A CN 110455952 A CN110455952 A CN 110455952A
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- Prior art keywords
- azo
- aromatic amine
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- food
- temperature
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The embodiment of the invention provides azo in a kind of food and aromatic amine compounds quick screening methods, include the following steps: step S1, sample pretreatment: the food samples for weighing specified wt are placed in test tube with cover, the citric acid sodium hydrate buffer solution of preheating is added into test tube with cover, it is stood in preset temperature water-bath after homogeneous, hydrogensulfite solution is added in centrifuging and taking supernatant, stands in preset temperature water-bath after being uniformly mixed, it is cooled to assigned temperature, obtains reaction solution；Step S2, sample separation and concentration: sodium hydroxide, sodium chloride and t-butyl methyl ether are added in the reaction solution, obtains extract liquor after shaking；Analysis detection: step S3 takes upper layer of extraction liquid using GC-MS measurement analysis, obtains the detection data of azo and aromatic amine.
Description
Technical field
The present invention relates to food technology fields, quick more particularly to azo in a kind of food and aromatic amine compounds
Screening method.
Background technique
Various pigment additives are widely used in food industry, in addition to GB 2760-2014 " national food safety standard food
Product additive uses standard " allow to limit other than the edible pigment used, it is also necessary to notice that industrial azo is illegally added in monitoring
The risk of class pigment.
Synthetic dyestuff is generally bright in colour, strong coloring force, and stability is good, and odorless, tasteless, quality is uniform, easy to dissolve and spelling
Color, and it is low in cost, it is widely used in the coloring of textile, leather, chemical industry, food, cosmetics etc..Currently to edible secondary colour
The safety issue of element is concentrated mainly on organic synthesis pigment, and the azo pigment in organic synthesis pigment can be in vivo
Generate mutagen precursor: aromatic amine compounds through metabolism, become after the further metabolism activation of aromatic amine electrophilic product with
DNA and RNA in conjunction with and Mutation induction；This property of azo substance have been identified as it is unsafe, have potential mistake
Quick reaction and carcinogenicity；Amaranth, famille rose, sunset yellow and lemon yellow etc. just belong to this kind of azopigments.
In addition in GB 2760-2014 " national food safety standard food additives use standard " regulation allow using
Edible pigment, at present it has also been found that generating the behavior that there is illegal addition azo pigment in enterprise, such as the tonyred announced
Illegal use of the class industry pigment in eggs products and flavouring；Wherein Sudan IV is metabolized in vivo can produce o- amino
Azotoluene 4- amino -2- tolyl azo-beta naphthal, 2,5- diaminotoluene, -2 naphthols of 1- amino and o- toluidines etc. is fragrant
Fragrant aminated compounds clearly proves there is carcinogenesis to human body, has apparent toxic effect to liver kidney.
In addition, azo pigment and related aromatic amine substance connect it is also possible to being present in printed matter in packaging material for food
Impurity in the migration stain and food additives generated is touched to bring into.
Currently, for azo and aromatic amine compounds rapid screening in food, the not no test method of clear stipulaties.
Summary of the invention
In view of the above problems, it proposes the embodiment of the present invention and overcomes the above problem or at least partly in order to provide one kind
Azo and aromatic amine compounds quick screening method in a kind of food to solve the above problems.
To solve the above-mentioned problems, the embodiment of the invention discloses azo in a kind of food and aromatic amine compounds are fast
Fast screening method, comprising:
Step S1, sample pretreatment: the food samples for weighing specified wt are placed in test tube with cover, are added into test tube with cover
The citric acid sodium hydrate buffer solution of preheating is stood in preset temperature water-bath after homogeneous, and Lian Erya is added in centrifuging and taking supernatant
Metabisulfite solution stands in preset temperature water-bath after being uniformly mixed, is cooled to assigned temperature, obtains reaction solution；Step S2,
Sample separation and concentration: sodium hydroxide, sodium chloride and t-butyl methyl ether are added in the reaction solution, is extracted after shaking
Take liquid；Analysis detection: step S3 takes upper layer of extraction liquid using GC-MS measurement analysis, obtains the detection of azo and aromatic amine
Data；
Further, the specified wt is 4.5~5.5g；The test tube with cover is 50mL；The hydrogen citrate oxidation
Sodium buffer is 25mL, and is preheated to 70 DEG C；The preset temperature is 68~72 DEG C；The water-bath time of repose be 29~
31min；The hydrogensulfite solution is 10mL；The cooling time is 2min；The assigned temperature is 20~25 DEG C；
Further, the step S2, comprising:
0.5mL40% sodium hydroxide solution and 7g sodium chloride are added in reaction solution, 5mL t-butyl methyl ether is added,
Extract liquor is obtained after shaking in shaking table；
Further, it is 14~16min that the time is shaken in the shaking table；
Further, the chromatographic condition of use: chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm；Injection port
Temperature: 220 DEG C；Carrier gas: helium；Flow rate of carrier gas is 2.48mL/min；Sample volume: 1 μ L；Splitless injecting samples；Temperature programming: described
Heating gradient is 60 DEG C of initial temperature, keeps 1min, is warming up to 150 DEG C with 15 DEG C/min, then be warming up to 320 DEG C with 20 DEG C/min, protects
It holds, 3min；Ion source temperature: 250 DEG C；Interface temperature: 250 DEG C；The Mass Spectrometry Conditions of use: full scan or selective scanning are used
Mode.
The embodiment of the present invention includes following advantages: detection lower bound is checked on and is established for the quality of consumer product up to 5mg/kg
Solid foundation；Using gas chromatography-mass spectrometry, complicated pretreatment process is eliminated, repeatability and reproducibility are more excellent, behaviour
Make easy；Remove from using a large amount of organic reagent, is conducive to environmental protection；GC-MS combines the high separation capacity and matter of chromatography
That composes is highly selective and highly sensitive, to establish micro and determination of trace accuracy basis；GC-MS the degree of automation
It is high, batch processing may be implemented, can be to the scientific analysis of result, to enormously simplify operation, improve detection work and imitate
Rate, while also improving the quality of analysis test job.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is aromatic amine standard substance curve graph；
Fig. 2 is aromatic amine standard substance chromatogram；
Fig. 3 is azo standard substance chromatogram.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with
Illustration illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
Azo and aromatic amine compounds quick screening method, include the following steps: in a kind of food of the invention
Step S1, sample pretreatment: the food samples for weighing specified wt are placed in test tube with cover, are added into test tube with cover
The citric acid sodium hydrate buffer solution of preheating is stood in preset temperature water-bath after homogeneous, and Lian Erya is added in centrifuging and taking supernatant
Metabisulfite solution stands in preset temperature water-bath after being uniformly mixed, is cooled to assigned temperature, obtains reaction solution；
Step S2, sample separation and concentration: sodium hydroxide, sodium chloride and tertbutyl methyl are added in the reaction solution
Ether obtains extract liquor after shaking；
Analysis detection: step S3 takes upper layer of extraction liquid using GC-MS measurement analysis, obtains azo and aromatic amine
Detection data.
Wherein in step 1, the specified wt is 4.5~5.5g；The test tube with cover is 50mL；The citric acid hydrogen-oxygen
Change sodium buffer is 25mL, and is preheated to 70 DEG C；The preset temperature is 68~72 DEG C；The water-bath time of repose be 29~
31min；The hydrogensulfite solution is 10mL；The cooling time is 2min；The assigned temperature is 20~25 DEG C.
Wherein in step S2,0.5mL40% sodium hydroxide solution and 7g sodium chloride are added in reaction solution, 5mL is added
T-butyl methyl ether obtains extract liquor after shaking in shaking table；It is 14~16min that the time is shaken in the shaking table.
Wherein in step S3, the Mass Spectrometry Conditions of the GC-MS are as follows:
The chromatographic condition of use: chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm；Injector temperature: 220
℃；Carrier gas: helium；Flow rate of carrier gas is 2.48mL/min；Sample volume: 1 μ L；Splitless injecting samples；Temperature programming: the heating gradient
It is 60 DEG C of initial temperature, keeps 1min, is warming up to 150 DEG C with 15 DEG C/min, then be warming up to 320 DEG C with 20 DEG C/min, keeps, 3min；
Ion source temperature: 250 DEG C；Interface temperature: 250 DEG C；
The Mass Spectrometry Conditions of use: full scan or selective scanning mode are used.
Embodiment one
Azo and aromatic amine compounds quick screening method, include the following steps: in a kind of food of the invention
Step S1, sample pretreatment: the candy sample for weighing 5g is placed in 50mL test tube with cover, is added into test tube with cover
25mL is preheated to 70 DEG C of citric acid sodium hydrate buffer solution, stands 30min, centrifuging and taking supernatant after homogeneous in 70 DEG C of water-bath
10mL hydrogensulfite solution is added in liquid, stands 30min in 70 DEG C of water-bath after being uniformly mixed, is cooled to 23 in 2min
DEG C, obtain reaction solution；
Wherein, citric acid sodium hydrate buffer solution is PH=6.
Step S2, sample separation and concentration: 0.5mL sodium hydroxide solution, 7g sodium chloride and 5mL are added in reaction solution
T-butyl methyl ether shakes 15min in shaking table, obtains extract liquor；
Wherein, it if cannot be layered completely, is centrifuged.
Analysis detection: step S3 takes upper layer of extraction liquid using GC-MS measurement analysis, obtains azo and aromatic amine
Detection data.
Sample liquid is analyzed immediately after being disposed, should be at -18 DEG C or less if analysis test cannot be completed interior for 24 hours
It is saved.
Wherein the Mass Spectrometry Conditions of the GC-MS are as follows:
The chromatographic condition of use: chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm；Injector temperature: 220
℃；Carrier gas: helium；Flow rate of carrier gas is 2.48mL/min；Sample volume: 1 μ L；Splitless injecting samples；Temperature programming: the heating gradient
It is 60 DEG C of initial temperature, keeps 1min, is warming up to 150 DEG C with 15 DEG C/min, then be warming up to 320 DEG C with 20 DEG C/min, keeps, 3min；
Ion source temperature: 250 DEG C；Interface temperature: 250 DEG C；The Mass Spectrometry Conditions of use: full scan or selective scanning mode are used.
It is tested by the detection of candy sample and mark-on reclaims, detects lower bound up to 5mg/kg.
Although the preferred embodiment of the embodiment of the present invention has been described, once a person skilled in the art knows bases
This creative concept, then additional changes and modifications can be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of range of embodiment of the invention.
Above to azo and aromatic amine compounds quick screening method in a kind of food provided by the present invention, carry out
It is discussed in detail, used herein a specific example illustrates the principle and implementation of the invention, above embodiments
Explanation be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art,
According to the thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion in this specification
Appearance should not be construed as limiting the invention.
Claims (5)
1. azo and aromatic amine compounds quick screening method in a kind of food characterized by comprising
Step S1, sample pretreatment: the food samples for weighing specified wt are placed in test tube with cover, and preheating is added into test tube with cover
Citric acid sodium hydrate buffer solution, stood in preset temperature water-bath after homogeneous, hydrosulfurous acid is added in centrifuging and taking supernatant
Sodium solution stands in preset temperature water-bath after being uniformly mixed, is cooled to assigned temperature, obtains reaction solution；
Step S2, sample separation and concentration: being added sodium hydroxide, sodium chloride and t-butyl methyl ether in the reaction solution,
Extract liquor is obtained after shaking；
Analysis detection: step S3 takes upper layer of extraction liquid using GC-MS measurement analysis, obtains the detection of azo and aromatic amine
Data.
2. azo and aromatic amine compounds quick screening method in food according to claim 1, which is characterized in that
The specified wt is 4.5~5.5g；The test tube with cover is 50mL；The citric acid sodium hydrate buffer solution is 25mL, and
It is preheated to 70 DEG C；The preset temperature is 68~72 DEG C；The water-bath time of repose is 29~31min；The hydrosulfurous acid
Sodium solution is 10mL；The cooling time is 2min；The assigned temperature is 20~25 DEG C.
3. azo and aromatic amine compounds quick screening method in food according to claim 1, which is characterized in that
The step S2, comprising:
0.5mL40% sodium hydroxide solution and 7g sodium chloride are added in reaction solution, 5mL t-butyl methyl ether is added, is shaking
Extract liquor is obtained after shaking in bed.
4. azo and aromatic amine compounds quick screening method in food according to claim 3, which is characterized in that
It is 14~16min that the time is shaken in the shaking table.
5. azo and aromatic amine compounds quick screening method in food according to claim 1, which is characterized in that
The Mass Spectrometry Conditions of the GC-MS are as follows:
The chromatographic condition of use: chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm；Injector temperature: 220 DEG C；It carries
Gas: helium；Flow rate of carrier gas is 2.48mL/min；Sample volume: 1 μ L；Splitless injecting samples；Temperature programming: the heating gradient is first
60 DEG C of temperature keeps 1min, is warming up to 150 DEG C with 15 DEG C/min, then be warming up to 320 DEG C with 20 DEG C/min, keeps 3min；Ion source
Temperature: 250 DEG C；Interface temperature: 250 DEG C；
The Mass Spectrometry Conditions of use: full scan or selective scanning mode are used.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910775447.9A CN110455952A (en) | 2019-08-21 | 2019-08-21 | Azo and aromatic amine compounds quick screening method in a kind of food |
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| CN201910775447.9A CN110455952A (en) | 2019-08-21 | 2019-08-21 | Azo and aromatic amine compounds quick screening method in a kind of food |
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| CN110455952A true CN110455952A (en) | 2019-11-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111721881A (en) * | 2020-07-07 | 2020-09-29 | 东莞诺威检测认证有限公司 | Trifluoroacetylation GC-MS (gas chromatography-mass spectrometry) detection method for banned azo dyes of textiles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111721881A (en) * | 2020-07-07 | 2020-09-29 | 东莞诺威检测认证有限公司 | Trifluoroacetylation GC-MS (gas chromatography-mass spectrometry) detection method for banned azo dyes of textiles |
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Application publication date: 20191115 |