CN110514752A - The extracting method of additive and its non-targeted screening method in a kind of paper food packaging materials - Google Patents
The extracting method of additive and its non-targeted screening method in a kind of paper food packaging materials Download PDFInfo
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- CN110514752A CN110514752A CN201910682713.3A CN201910682713A CN110514752A CN 110514752 A CN110514752 A CN 110514752A CN 201910682713 A CN201910682713 A CN 201910682713A CN 110514752 A CN110514752 A CN 110514752A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
Abstract
The invention discloses a kind of extracting methods of additive in paper food packaging materials, comprising the following steps: (1) weighs Noryl, be laid in weighing disk bottom；(2) part paper food packaging materials packaged food region is cut as sample, and sample is laid on Noryl, gland sealing；(3) weighing disk containing sample and Noryl in step (2) is placed in baking oven and carries out migration test；(4) Noryl in weighing disk is transferred in centrifuge tube, is centrifuged after ultrasonic wave extraction, supernatant liquor is transferred to nitrogen in concentrate bottle and blows concentration, the additive extract of sample is obtained after organic membrane filtration.The present invention further discloses a kind of non-targeted screening methods of additive in paper food packaging materials, screening method specificity of the present invention is strong, it is easy to operate, quick and precisely, analysis type it is abundant, can quickly analyze to control with quality for paper food packaging materials scientific method is provided.
Description
Technical field
The invention belongs to food packaging technical field of analysis and detection, and in particular to add in a kind of paper food packaging materials
The extracting method of agent and its non-targeted screening method.
Background technique
A large amount of appearance of poisonous and harmful food in recent years have caused the public and the extreme of food safety have been distrusted, with this
The closely related packaging material for food of food safety is also in the visual field for gradually coming into the public simultaneously.Along with the pressure of environmental protection, closely
It is plastics and papery that packaging material for food is most commonly used over year, and wherein paper wrapper has good recyclability, can be complete
It meets environmental requirements, therefore is widely used entirely, furthermore paper wrapper also has in terms of processing performance and mechanical strength
Excellent performance.Paper wrapper can carry out a series of processing, according to the package design of product during use
Need to add some such as fungicide, curing agent, brightening agent in process, these additives have potential danger, and having can
It can move in food, harm is generated to the health of human body of consumer.In order to study these additives for the shadow of food safety
It rings, it is necessary to establish analyzing detecting method quickly, accurate, easy.
Non-targeted screening measuring method reported at present is frequently with gas chromatography and liquid chromatography/mass spectrometry method
The specificity for guaranteeing detection method, mostly uses tandem mass spectrometry.Based on having for liquid chromatography-mass spectrometry (LC-MS)
Although machine object quantitative analysis method high sensitivity, be usually be directed to certain or certain substance, cause many unknown organic matters without
Method is found in time.Therefore, it needs to establish quick, simple organic matter screening method.Gas chromatography-mass spectrum GC-MS is chemical combination
One of common analytical technology of object Structural Identification, the technology can provide compound structure information and molecular weight information abundant, have
Conducive to compound structure identification, while there are also NIST standard database for reference.
However, complicated component in paper food packaging materials, wherein the interference impurity in addition to object (additive) is not
Only can jamming target object analysis, can also cause fatal damage to the chromatographic column in the gentle phase chromatography of mass spectrum, therefore how effectively
Extract paper food packaging materials in additive and purify removal paper food packaging materials in interference impurity become need to solve
A problem certainly.
In order to solve problem above, the present invention is proposed.
Summary of the invention
First aspect present invention provides a kind of extracting method of additive in paper food packaging materials, including following step
It is rapid:
(1) Noryl is weighed, weighing disk bottom is laid in；
(2) cutting part paper food packaging materials packaged food region as sample interception area is 0.385-
0.435dm2, sample is laid on Noryl, gland sealing, sample contacts food side is poly- towards the modification
Phenylate；
(3) weighing disk containing sample and Noryl in step (2) is placed in 70-90 DEG C of baking oven and carries out migration examination
It tests, is taken out after 2-4h, cooled to room temperature；It is highly preferred that by the weighing disk in step (2) containing sample and Noryl
It is placed in 70 DEG C of baking ovens and carries out migration test, taken out after 2h；
(4) Noryl in weighing disk is fully transferred in 50mL centrifuge tube, 10-20mL ethyl alcohol, ultrasound is added
Wave is centrifuged after extracting, and supernatant liquor is fully transferred in concentrate bottle, and nitrogen, which is blown, under 40-60 DEG C of water bath condition is concentrated into 1-2mL,
The additive extract of sample is obtained after 0.45 μm of organic membrane filtration.Wherein organic filter membrane is that laboratory commonly can be resistance to
The miillpore filter of organic solvent.
Wherein, in step (2) and step (3), Noryl (MPPO) is solid particle, sample is laid in modified poly-
On phenylate, gland sealing, and sample contacts food side, towards the Noryl, Noryl can adsorb papery
Additive in packaging material for food, to complete to move to the additive in paper food packaging materials in Noryl
The step of, then with ethanol solution to solvent extraction is carried out in Noryl, to guarantee that extract does not have papery packaging for foodstuff material
Interference impurity in material, avoid directly adopt in the prior art ethanol solution to paper food packaging materials carry out solvent mention
It takes, includes not only additive to be measured in caused extract, further include the interference impurity in a large amount of paper food packaging materials.
Preferably, ultrasonic frequency is 2000-4000Hz, ultrasonic time 10-20min in the step (4)；Centrifugation turns
Speed is 2000-4000rpm, centrifugation time 5min.
Second aspect of the present invention provides a kind of non-targeted screening method of additive in paper food packaging materials, including with
Lower step:
(1) the additive extract for the sample that the extracting method provided according to a first aspect of the present invention obtains is as to be measured
Object, the additive in determinand is as object；
(2) gas chromatography-mass spectrum detects: using HP-5MS chromatographic column as separation means, in monitoring mass number range 29-
The full scan mode of 550amu detects determinand；
(3) substance qualitative and quantitative analysis: to it is to be measured look for spectral peak to carry out background deduction after, using NIST library searching, protect
The qualitative results that spectrum storehouse matching degree is higher than 70% are stayed and record, when finding unlicensed additive in qualitative results, using described
The standard items of unlicensed additive carry out qualitative confirmation；Quantitative approach is internal standard method；
(4) object relative amount calculates in sample: object relative amount X is calculated by formula (1) in sample:
X=(As-A0) * Ci*V*f/ (Ai*S) ... ... ... ... ... ... ... (1)
In formula:
X-object relative amount, unit mg/m2；
As-object peak area
A0-blank control sample peak area
Ai-internal standard compound peak area
Ci-internal standard compound concentration, unit ug/mL
V-internal standard compound volume, unit mL
Cycles of concentration in f-step (1)
The interception area of paper food packaging materials, unit m in S-step (1)2。
Wherein, blank control sample does not have in the extraction process of additive in paper food packaging materials in step (1)
There is the alcohol solvent that paper food packaging materials sample and Noryl is added, i.e., without extracting paper food packaging materials examination
The alcohol solvent sample of additive in sample.
Preferably, the internal standard compound that the internal standard method is selected is deuterated anthracene, and 100 μ L are added in determinand in step (1)
The acetonitrile inner mark solution of deuterated anthracene.The preparation method of the acetonitrile inner mark solution of deuterated anthracene: the deuterated anthracene of 10mg is accurately weighed, accurately
To 0.1mg, with acetonitrile dissolution and constant volume is in 100mL volumetric flask, and it is molten to be configured to the deuterated anthracene internal standard that concentration is 100 μ g/mL
Liquid, seals stored protected from light under the conditions of 0~4 DEG C, and validity period 3 months.
Preferably, chromatographic condition in gas chromatograph-mass spectrometer (GC-MS) in step (2) are as follows: chromatographic column is HP-5MS capillary
Chromatographic column, specification are 30m × 0.25mm × 0.25 μm；Carrier gas is high-purity helium He, constant current mode, flow velocity 1.0mL/min；Into
Sample mouth temperature is 290 DEG C；1 μ L of sample volume, Splitless injecting samples；Temperature programming condition is that initial temperature is 70 DEG C, keeps 3min, with
The rate of 10 DEG C/min rises to 290 DEG C, keeps 5min.
Preferably, Mass Spectrometry Conditions in gas chromatograph-mass spectrometer (GC-MS) in step (2) are as follows: EI ionizes mode, ionization energy
70eV, 230 DEG C of ion source temperature, 150 DEG C of quadrupole rod temperature；Scanning mode is full scan mode, mass number range 29-
550amu；Solvent delay 3min.
Preferably, qualitative analysis step in step (3): first to chromatographic peak carry out background deduction, according to appearance reservation when
Between, using NIST library searching, retain and record the qualitative results that spectrum storehouse matching degree is higher than 70%, for retrieval by header discovery
Doubtful unlicensed substance needs to carry out qualitative confirmation using standard items.The selection ion chromatography peak of sample prepare liquid and standard items
(± 0.1min) occurs at identical retention time, and quota ion and the mass-to-charge ratio and standard items one that assist qualitative ion
It causes, abundance ratio should meet with standard items compared with: when relative abundance > 50%, ± 10% deviation of permission；Relative abundance 20%~
When 50%, allow ± 15% deviation；When relative abundance 10%~20%, allow ± 20% deviation；When relative abundance≤10%, permit
Perhaps ± 50% deviation, at this time can qualitative discrimination target analytes.
Quantitative analysis step: take respectively series standard working solution carry out GC-MS analysis, with each standard working solution with it is interior
The ratio for marking the quota ion peak area of object is ordinate, using the content of each standard working solution as abscissa, draws standard work
Make curve, working curve linearly dependent coefficient R2>0.99.Look for spectral peak area for reference with internal standard, by qualitative substance color out
In spectral peak area standard curve corresponding with the substitution of reference peak area ratio, the qualitative corresponding content of the substance out can be obtained.
Compared with the existing technology, the invention has the following advantages:
1, extracting method of the invention is the transportable substance (additive) trapped in paper food packaging materials first, so
The transportable object trapped afterwards with solvent extraction, this method can avoid extract paper food packaging materials in other interference it is miscellaneous
The additive in paper food packaging materials is effectively extracted under the premise of matter, compared with the existing technology in directly pass through solvent extract
The method taken extracts the additive in paper food packaging materials, and extracting method of the present invention more quick and precisely, can not only have
Effect extracts the additive in paper food packaging materials, also avoids other in paper food packaging materials during subsequent screening
It is damaged caused by chromatographic column in interference impurity mass spectrum and gas-chromatography.
2, it the present invention provides a kind of non-targeted quick screening method of additive in paper food packaging materials, mentions first
Additive in paper food packaging materials is taken, then using deuterated anthracene as internal standard compound, using gas-chromatography-Mass Spectrometry (GC/
MS object relative amount in sample) is measured, the method for the present invention Screening analysis paper food packaging materials specificity is strong, operation is simple
It is single, quick and precisely, analysis type it is abundant, can quickly analyze to control with quality for paper food packaging materials scientific method is provided.
Detailed description of the invention
Fig. 1 paper food packaging materials sample screening chromatogram of the embodiment of the present invention.
Specific embodiment
Of the invention for ease of understanding, below with reference to specific embodiment, the technical scheme of the present invention will be further described.
It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.
Reagent and drug used in the present embodiment:
Noryl (MPPO, the entitled Tenax-TA adsorbent of convenience goods)；Acetonitrile, chromatographically pure；Water, GB/T
6682, level-one；Deuterated anthracene (C14D10, CAS:1719-06-8), purity >=98%；Inner mark solution accurately weighs the deuterated anthracene of 10mg,
It is accurate to 0.1mg, with acetonitrile dissolution and constant volume is in 100mL volumetric flask, is configured to the deuterated anthracene internal standard that concentration is 100 μ g/mL
Solution, seals stored protected from light under the conditions of 0~4 DEG C, and validity period 3 months.
Instrument and material used in the present embodiment:
Gas chromatograph-mass spectrometer (GC-MS) (GC-MS)；Assay balance, sensibility reciprocal 0.1mg；Weighing disk, specification 70mm ×
35mm；Centrifuge tube, 15mL, 50mL；Piston type liquid-transfering gun, 1000 μ L；Conical flask 100mL, band cock；Concentrate bottle, 50mL.
The present embodiment is a kind of non-targeted screening method of additive in paper food packaging materials, comprising the following steps:
(1) determinand extracts in paper food packaging materials
1g ± 0.0001g MPPO is accurately weighed, it is evenly laid out in weighing disk bottom；Cut food papery packaging for foodstuff material
Packaged food region is expected as sample, and cutting region area is 0.385dm2(diameter 70mm).Sample is laid on MPPO, is pressed
Lid sealing, sample contacts food side is towards the Noryl.Weighing disk containing sample is placed in 70 DEG C of baking ovens
Middle carry out migration test is taken out after 2h, cooled to room temperature.MPPO in weighing disk is fully transferred to 50mL centrifuge tube
In, the deuterated anthracene acetonitrile inner mark solution of 100 μ L and 20mL ethyl alcohol, ultrasonic wave extraction 20min, under the conditions of 4000rpm are added respectively
It is centrifugated 5min, supernatant liquor is fully transferred in concentrate bottle, and nitrogen, which is blown, under 40 DEG C of water bath conditions is concentrated into 1mL, warp
GC-MS analysis is carried out after 0.45 μm of organic phase filter membrane filtering.
(2) gas chromatograph-mass spectrometer (GC-MS) detects
Prepare liquid is separated by liquid chromatographic system, chromatographic condition: chromatographic column: capillary chromatographic column, stationary phase are
(5% phenyl)-methyl polysiloxane, specification are [30m (length) × 0.25mm (internal diameter) × 0.25 μm (film thickness)]；Carrier gas: high
Pure helium (He), constant current mode, flow velocity 1.0mL/min；Injector temperature: 290 DEG C；1 μ L of sample volume, Splitless injecting samples；Journey
Sequence heating: initial temperature is 70 DEG C, keeps 3min, rises to 290 DEG C with the rate of 10 DEG C/min, keeps 5min.Mass spectrum refers to item
Part is as follows: EI ionization mode, ionization energy 70eV, and 230 DEG C of ion source temperature, 150 DEG C of quadrupole rod temperature；Scanning mode: full scan
Mode, mass number range 29-550amu；Solvent delay: 3min.
Wherein, the present embodiment paper food packaging materials sample screening chromatogram is shown in Fig. 1.
(3) substance qualitative, quantitative
After carrying out background deduction to chromatographic peak, using NIST library searching, retains and record spectrum storehouse matching degree higher than 70%
Qualitative results；For the doubtful unlicensed substance of retrieval by header discovery, need to carry out qualitative confirmation using standard items.Sample waits for
The selection ion chromatography peak of liquid and standard items at identical retention time (± 0.1min) is surveyed to occur, and quota ion with it is auxiliary
It helps the mass-to-charge ratio of qualitative ion consistent with standard items, abundance ratio should meet compared with standard items: when relative abundance > 50%, permitting
Perhaps ± 10% deviation；When relative abundance 20%~50%, allow ± 15% deviation；When relative abundance 10%~20%, allow ±
20% deviation；When relative abundance≤10%, allow ± 50% deviation, it at this time can qualitative discrimination target analytes.
19, the peak of identifiable object in this prepare liquid chromatogram, table 1 are the GC-MS of 19 kinds of objects of record
Parameter.
For 19 kinds of substances out qualitative in above-mentioned steps, mass concentration gradient is purchased respectively are as follows: 500ng/mL,
The standard working solution of 200ng/mL, 100ng/mL, 50ng/mL, 20ng/mL, and standard working solution is injected into gas-chromatography-
Mass spectrometer is measured, for each qualitative substance, with the quota ion peak of each standard working solution and internal standard compound
The ratio of area is ordinate, using the content of each standard working solution as abscissa, draws standard working curve, working curve line
Property coefficient R2>0.99.Look for spectral peak area for reference with internal standard, by qualitative substance chromatographic peak area and reference peak face out
The ratio between product substitutes into corresponding standard curve, and the qualitative corresponding content of the substance out can be obtained.
The GC-MS parameter of 1 19 kinds of objects of table
(4) relative amount of object calculates in sample
The relative amount (X) of object is calculated by formula (1) in paper food packaging materials sample:
X=(As-A0) * Ci*V*f/ (Ai*S) ... ... ... ... ... ... ... (1)
In formula:
X-object relative amount (mg/m2)
As-object peak area
A0-blank control sample peak area
The interior target peak area of Ai-
The interior target concentration (ug/mL) of Ci-
The interior target volume (mL) of V-
Cycles of concentration in f-step (1)
Interception area (the m of paper food packaging materials in S-step (1)2)
Wherein, blank control sample does not have in the extraction process of additive in paper food packaging materials in step (1)
There is the alcohol solvent that paper food packaging materials sample and Noryl is added, i.e., without extracting paper food packaging materials examination
The alcohol solvent sample of additive in sample.
Calculate separately the relative amount summary sheet 2 of identifiable 19 objects in this prepare liquid.
Relative amount of the 2 19 kinds of objects of table in paper food packaging materials
Claims (8)
1. the extracting method of additive in a kind of paper food packaging materials, which comprises the following steps:
(1) Noryl is weighed, weighing disk bottom is laid in；
(2) part paper food packaging materials packaged food region is cut as sample, and sample is laid on Noryl,
Gland sealing, sample contacts food side is towards the Noryl；
(3) weighing disk containing sample and Noryl in step (2) is placed in baking oven and is migrated, is cooled to after taking-up
Room temperature；
(4) Noryl in weighing disk is fully transferred in centrifuge tube, alcohol solvent is added, after ultrasonic wave extraction from
Supernatant liquor after centrifugation is fully transferred in concentrate bottle by the heart, and nitrogen blows concentration under water bath condition, after organic membrane filtration
To the additive extract of paper food packaging materials.
2. extracting method according to claim 1, which is characterized in that cut part papery food packet in the step (2)
As sample, interception area is 0.385-0.435dm in package material packaged food region2。
3. extracting method according to claim 1, which is characterized in that oven temperature is 70-90 DEG C in the step (3),
Transit time is 2-4h.
4. extracting method according to claim 1, which is characterized in that 10-20mL ethyl alcohol is added in the step (4), surpasses
Sound wave is centrifuged after extracting, and supernatant liquor after centrifugation is fully transferred in concentrate bottle, nitrogen blows concentration under 40-60 DEG C of water bath condition
To 1-2mL；Ultrasonic frequency is 2000-4000Hz, ultrasonic time 10-20min；Centrifugal rotational speed is 2000-4000rpm, from
The heart time is 5min；Organic filter membrane is 0.45 μm of organic filter membrane.
5. the non-targeted screening method of additive in a kind of paper food packaging materials, which comprises the following steps:
(1) prepared by determinand: the additive extract of paper food packaging materials is made in the method according to claim 1, by it
As determinand, the additive in determinand is as object；
(2) gas chromatography-mass spectrum detects: using HP-5MS chromatographic column as separation means, in monitoring mass number range 29-550amu
Full scan mode determinand is detected；
(3) object qualitative and quantitative analysis: to it is to be measured look for spectral peak to carry out background deduction after, using NIST library searching, retain
And the qualitative results that spectrum storehouse matching degree is higher than 70% are recorded, when finding unlicensed additive in qualitative results, using described non-
The standard items of additive are permitted to carry out qualitative confirmation；Quantitative approach is internal standard method；
(4) relative amount of object in paper food packaging materials, object phase in the paper food packaging materials are calculated
Content X is calculated by formula (1):
X=(As-A0) * Ci*V*f/ (Ai*S) ... ... ... ... ... ... ... (1)
In formula:
X-object relative amount, unit mg/m2；
As-object peak area
A0-blank control sample peak area
Ai-internal standard compound peak area
Ci-internal standard compound concentration, unit ug/mL
V-internal standard compound volume, unit mL
Cycles of concentration in f-step (1)
The interception area of paper food packaging materials, unit m in S-step (1)2。
6. screening method according to claim 3, which is characterized in that the internal standard compound that the internal standard method is selected is deuterated anthracene.
7. screening method according to claim 3, which is characterized in that color in gas chromatograph-mass spectrometer (GC-MS) in step (2)
Spectral condition are as follows: chromatographic column is HP-5MS capillary chromatographic column, and specification is 30m × 0.25mm × 0.25 μm；Carrier gas is high-purity helium
He, constant current mode, flow velocity 1.0mL/min；Injector temperature is 290 DEG C；1 μ L of sample volume, Splitless injecting samples；Temperature programming item
Part is that initial temperature is 70 DEG C, keeps 3min, rises to 290 DEG C with the rate of 10 DEG C/min, keeps 5min.
8. screening method according to claim 3, which is characterized in that matter in gas chromatograph-mass spectrometer (GC-MS) in step (2)
Spectral condition are as follows: EI ionization mode, ionization energy 70eV, 230 DEG C of ion source temperature, 150 DEG C of quadrupole rod temperature；Scanning mode is to sweep entirely
Retouch mode, mass number range 29-550amu；Solvent delay 3min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112924595A (en) * | 2021-01-27 | 2021-06-08 | 上海烟草集团有限责任公司 | Method for detecting acrylic resin monomer migration volume in paper packaging material |
| CN113030299A (en) * | 2021-02-22 | 2021-06-25 | 广州海关技术中心 | Method for screening and evaluating safety of unintended or intended additive migration amount in recycled PET (polyethylene terephthalate) product for food contact |
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