CN105588910B - The methods of risk assessment that plastic products migration thing influences on wine product - Google Patents
The methods of risk assessment that plastic products migration thing influences on wine product Download PDFInfo
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- CN105588910B CN105588910B CN201510940831.1A CN201510940831A CN105588910B CN 105588910 B CN105588910 B CN 105588910B CN 201510940831 A CN201510940831 A CN 201510940831A CN 105588910 B CN105588910 B CN 105588910B
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
The invention belongs to chemical analysis and food safety risk evaluation areas, and in particular to one kind wine brewing production migrates thing with plastic products influences methods of risk assessment to wine product.The technical problems to be solved by the invention are to provide the methods of risk assessment that a kind of production plastic products migration thing of making wine influences on wine product, comprise the following steps:A, plastic products are crushed after be added in treatment fluid, place under simulated conditions extract, filtering, obtain filtrate, as leaching liquor;Described treatment fluid is any one in wine product or analogies;B, with GC MS, LC QTOF, ICP MS leaching liquor and treatment fluid are detected respectively, the spectrogram for passing through leaching liquor and treatment fluid is contrasted, it was therefore concluded that.This method can comprehensively detect that plastic products move to the various materials in wine or vinasse, accurate, conveniently, and then be estimated, and be that wine product has safely provided more preferably more fully methods of risk assessment.
Description
Technical field
The invention belongs to chemical analysis and food safety risk evaluation areas, and in particular to a kind of plastic products migrate thing pair
The methods of risk assessment of wine product influence.
Background technology
Current China lacks sufficiently research to the safety issue of packaging material for food and assessed, and is especially the absence of to food
The safety evaluatio related art method of important harmful substance, not yet sets up nuisance in packaging material for food in product packaging material
The Safety Assessment System of matter, is not more directed to the appraisal procedure of this Special food of white wine, and white wine is crossed in also nobody's system research
The migration problem of compound in manufacturing enterprise's plastic products, in terms of only report is also plasticiser.
In order to make up deficiency of the national standard in terms of food packaging material risk assessment, it is to avoid similar wine product " modeling
The generation again of agent event ", we have proposed a kind of brand-new appraisal procedure, that is, production of making wine migrates thing with plastic products
The high-flux detection method of non-targeted compound.This method can be detected to the migration thing in be likely to enter wine, be entered
And be estimated, and be in terms of product safety and product quality two.
Inductivity coupled plasma mass spectrometry (ICP-MS) detection sensitivity under full scan state, which reaches, flies gram level, as long as entering
Enter the activated energy in wine and reach that harmful concentration is absolutely detected.Liquid chromatogram-level Four bar flight
Time mass spectrum combined instrument (LC-QTOF) is very high to heterocyclic compound sensitivity under holotype, to organic acid, phenol under negative mode
Deng sensitivity it is very high, Gamma Magnitude can be reached, harmful organic compound content is generally all micro-
It is more than gram level.Gas chromatograph-mass spectrometer (GC-MS) can also reach milligram level to the detection sensitivity of organic matter, substantially meet need
Will.Sensitivity of the sense organ of people to aroma compound is often higher than instrument and equipment, has in conjunction with as defined in organoleptic detection and standard
The detection of the harmful migration thing of poison, can comprehensive assessment plastic products migration thing to the quality of wine product and have impact on for safety.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of plastic products migration thing and the risk that wine product influences are commented
Estimate method.This method comprises the following steps:
A, plastic products are crushed after be added in treatment fluid, place under simulated conditions extract, filtering, obtain filtrate, i.e.,
For leaching liquor;Described treatment fluid is any one in wine product or analogies;
B, with GC-MS, LC-QTOF, ICP-MS leaching liquor and treatment fluid are detected respectively, pass through the spectrum of leaching liquor and treatment fluid
Figure contrast, it was therefore concluded that.
Specifically, in above-mentioned methods of risk assessment step a, plastic products are crushed into individual particle≤0.02g, mixing is equal
It is even, 2~5g is weighed, is added in 50mL treatment fluids, is put under simulated conditions and extracts, filtering obtains filtrate, as leaching liquor.
Specifically, in above-mentioned methods of risk assessment step a, described simulated conditions are 40 DEG C ± 1 DEG C of soaking temperature, immersion
Time 10d.
Specifically, in above-mentioned methods of risk assessment step a, described analogies are analogies A, spirituosity 4~6%, second
The aqueous solution of acid 4~6%.
Specifically, in above-mentioned methods of risk assessment step a, described analogies are analogies B, spirituosity 50~70%,
The aqueous solution of acetic acid 0.5~1%.
Specifically, in above-mentioned methods of risk assessment step a, described analogies are analogies C, containing 90~100% alcohol.
It is preferred that, in above-mentioned methods of risk assessment step a, when detecting influence of the plastic products migration thing to vinasse, institute
The wine product stated is the distillate that vinasse are added after water distillation;Described analogies are analogies A.
It is preferred that, in above-mentioned methods of risk assessment step a, when detecting influence of the plastic products migration thing to finished wine,
Described wine product is finished wine;Described analogies are at least one of analogies B or analogies C.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the GC-MS are:GC testing conditions are:Rise
Warm program:40 DEG C of holding 5min, are warming up to 220 DEG C of holding 10min, then be warming up to 280 DEG C of holdings with 5 DEG C/min with 4 DEG C/min
5min;Or 40 DEG C of holding 1min, 220 DEG C of holding 1min are warming up to 6 DEG C/min, then 280 DEG C of holdings are warming up to 5 DEG C/min
5min;Sample size:1~5uL;Input mode:Splitless injecting samples.
Further, in above-mentioned methods of risk assessment step b, the testing conditions of the GC-MS are:GC detections are used
Gas chromatographic column is:HPINWAX 60m*0.25mm*0.25 μm or HP-5Agilent30m*0.25mm*0.25 μm.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the GC-MS are:MS testing conditions are:Electricity
From mode:EI;Scan mode:Full scan;Ionizing energy:70ev;Mass scan range:30~550.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the LC-QTOF are:LC testing conditions are:
Mobile phase:Methanol B, ultra-pure water A;Gradient elution:0~12min:10%B~100%B, 12min~20min:100%B,
20min~22min:100%B~10%B, 22min:Stop;Column temperature:20~30 DEG C;Flow velocity:0.1~0.3mL/min;Sample introduction
Volume:1~5uL.
Further, in above-mentioned methods of risk assessment step b, the testing conditions of the LC-QTOF are:LC detections are used
Chromatographic column be:Agilent Eclipse Plus C18 2.1*50mm 1.8-micron.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the LC-QTOF are:QTOF testing conditions
For:Ion gun:DESI sources;The holotype condition of scanning:Dry temperature degree:300℃;Dry gas stream amount:10L/min;Atomizer pressure
Power:40psig;Capillary voltage:4000v;Capillary outlet voltage:60v;The negative mode condition of scanning:Dry temperature degree:300
℃;Dry gas stream amount:8L/min;Nebulizer pressure:40psig;Capillary voltage:3500v;Capillary outlet voltage:60v.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the ICP-MS are:Scan pattern:Sweep entirely
Retouch;Scanning times:100;Forward power:1400W;Residence time:10000μs;Sampling time:13s;Sampling depth:
159step;Cooling gas flow:13.0L/min;Secondary air amount:0.70L/min;Atomization gas flow:0.95L/min;Peristaltic pump
Rotating speed:25r/min;Number of repetition:3.
The mode that the inventive method is combined by using tri- kinds of equipment of GC-MS, LC-QTOF, ICP-MS, have selected and respectively set
Standby suitable testing conditions, with reference to the dissolution situation of plastic products respectively in wine product and analogies, can more accurately sentence
The dissolution situation of disconnected organic matter and inorganic matter of the plastic products in wine product, so as to more accurately judge that plastic products are produced in wine
The risk situation in product field.Meanwhile, the migration situation of migration thing of the plastic products in analogies can be true in the inventive method
Migration situation of the real reflection plastic products migration thing in wine product, can save detection plastic products and migrate thing in various differences
The migration situation of wine product, so as to provide a reliable mark to migrate influence of the thing to wine in plastic products in wine industry
It is accurate.
Brief description of the drawings
The GC-MS figures of PVC leaching liquors of gained in analogies B in Fig. 1 embodiments 1
The GC-MS figures of analogies B in Fig. 2 embodiments 1
The GC-MS figures of PVC leaching liquors of gained in analogies C in Fig. 3 embodiments 1
The GC-MS figures of analogies C in Fig. 4 embodiments 1
The GC-MS figures of PVC leaching liquors of gained in five-Grain Liquor base liquor in Fig. 5 embodiments 1
The GC-MS figures of five-Grain Liquor base liquor in Fig. 6 embodiments 1
The GC-MS figures of PVC leaching liquors of gained in Maotai in Fig. 7 embodiments 1
The GC-MS figures of Maotai in Fig. 8 embodiments 1
The GC-MS figures of PVC leaching liquors of gained in Fenyang wine in Fig. 9 embodiments 1
The GC-MS figures of Fenyang wine in Figure 10 embodiments 1
The upper figures of Figure 11 are LC-QTOF figures of the analogies B under holotype in embodiment 1;Figure below is PVC in analogies B
LC-QTOF figure of the leaching liquor of gained under holotype
The upper figures of Figure 12 are the LC-QTOF figures of analogies B in negative mode in embodiment 1;Figure below is PVC in analogies B
The LC-QTOF figures of the leaching liquor of gained in negative mode
The upper figures of Figure 13 are LC-QTOF figures of the analogies C under holotype in embodiment 1;Figure below is PVC in analogies C
LC-QTOF figure of the leaching liquor of gained under holotype
The upper figures of Figure 14 are LC-QTOF figures of the analogies C under holotype in embodiment 1;Figure below is PVC in analogies C
The LC-QTOF figures of the leaching liquor of gained in negative mode
The upper figures of Figure 15 are LC-QTOF figure of the five-Grain Liquor base liquor under holotype in embodiment 1;Figure below is in embodiment 1
PVC in five-Grain Liquor base liquor gained leaching liquor under holotype LC-QTOF figure
The upper figures of Figure 16 are the LC-QTOF figures of five-Grain Liquor base liquor in negative mode in embodiment 1;Figure below is in embodiment 1
PVC in five-Grain Liquor base liquor gained leaching liquor in negative mode LC-QTOF figure
The upper figures of Figure 17 are LC-QTOF figure of the Maotai under holotype in embodiment 1;Figure below be embodiment 1 in PVC in
LC-QTOF figure of the gained leaching liquor under holotype in Maotai
The upper figures of Figure 18 are the LC-QTOF figures of Maotai in negative mode in embodiment 1;Figure below be embodiment 1 in PVC in
The LC-QTOF figures of gained leaching liquor in negative mode in Maotai
The upper figures of Figure 19 are LC-QTOF figure of the Fenyang wine under holotype in embodiment 1;Figure below is the PVC in embodiment 1 in Fen
LC-QTOF figure of the gained leaching liquor under holotype in wine
The upper figures of Figure 20 are the LC-QTOF figures of Fenyang wine in negative mode in embodiment 1;Figure below is the PVC in embodiment 1 in Fen
The LC-QTOF figures of gained leaching liquor in negative mode in wine
The ICP-MS figures of PVC gained leaching liquors in analogies B in Figure 21 embodiments 1
Analogies B ICP-MS figures in Figure 22 embodiments 1
The ICP-MS figures of PVC gained leaching liquors in analogies C in Figure 23 embodiments 1
Analogies C ICP-MS figures in Figure 24 embodiments 1
The ICP-MS figures of PVC leaching liquors of gained in five-Grain Liquor base liquor in Figure 25 embodiments 1
The ICP-MS figures of five-Grain Liquor base liquor in Figure 26 embodiments 1
The ICP-MS figures of PVC leaching liquors of gained in Maotai in Figure 27 embodiments 1
The ICP-MS figures of Maotai in Figure 28 embodiments 1
The ICP-MS figures of PVC leaching liquors of gained in Fenyang wine in Figure 29 embodiments 1
The ICP-MS figures of Fenyang wine in Figure 30 embodiments 1
The GC-MS figures that vinasse steam wine sample are put up in Figure 31 embodiments 2 with PE plastic clothes
Unused PE plastic clothes put up the GC-MS figures that vinasse steam wine sample in Figure 32 embodiments 2
PE plastics are distributed in the GC-MS figures of gained leaching liquor in analogies A in Figure 33 embodiments 2
Analogies A GC-MS figures in Figure 34 embodiments 2
The upper figures of Figure 35 are that unused PE plastic clothes put up the LC-QTOF of wine sample that vinasse steam under holotype in embodiment 2
Figure;Figure below steams LC-QTOF figure of the wine sample under holotype to put up vinasse in embodiment 2 with PE plastic clothes
The upper figures of Figure 36 are that unused PE plastic clothes put up vinasse and steam to obtain the LC-QTOF of wine sample in negative mode in embodiment 2
Figure;Figure below steams the LC-QTOF figures of wine sample in negative mode to put up vinasse in embodiment 2 with PE plastic clothes
The upper figures of Figure 37 are LC-QTOF figures of the analogies A under holotype in embodiment 2;Figure below is PE plastics in embodiment 2
Gained leaching liquor in analogies A is distributed in the LC-QTOF of holotype to scheme
The upper figures of Figure 38 are the LC-QTOF figures of analogies A in negative mode in embodiment 2;Figure below is PE plastics in embodiment 2
Gained leaching liquor in analogies A is distributed in the LC-QTOF of negative mode to scheme
The ICP-MS figures that vinasse steam wine sample are put up in Figure 39 embodiments 2 with PE plastic clothes
Unused PE plastic clothes put up the ICP-MS figures that vinasse steam wine sample in Figure 40 embodiments 2
PE plastics are distributed in the ICP-MS figures of gained leaching liquor in analogies A in Figure 41 embodiments 2
Analogies A ICP-MS figures in Figure 42 embodiments 2
Embodiment
The methods of risk assessment that a kind of plastic products migration thing influences on wine product, comprises the following steps:
A, plastic products are crushed after be added in treatment fluid, place under simulated conditions extract, filtering, obtain filtrate, i.e.,
For leaching liquor;Described treatment fluid is any one in wine product or analogies;
B, with GC-MS, LC-QTOF, ICP-MS leaching liquor and treatment fluid are detected respectively, pass through the spectrum of leaching liquor and treatment fluid
Figure contrast, it was therefore concluded that.
Specifically, in above-mentioned methods of risk assessment step a, plastic products are crushed into individual particle≤0.02g, mixing is equal
It is even, 2~5g is weighed, is added in 50mL treatment fluids, is put under simulated conditions and extracts, filtering obtains filtrate, as leaching liquor.
Specifically, in above-mentioned methods of risk assessment step a, described simulated conditions are 40 DEG C ± 1 DEG C of soaking temperature, immersion
Time 10d.
Specifically, in above-mentioned methods of risk assessment step a, described analogies are analogies A, spirituosity 4~6%, second
The aqueous solution of acid 4~6%.
Specifically, in above-mentioned methods of risk assessment step a, described analogies are analogies B, spirituosity 50~70%,
The aqueous solution of acetic acid 0.5~1%.
Specifically, in above-mentioned methods of risk assessment step a, described analogies are analogies C, containing 90~100% alcohol.
It is preferred that, in above-mentioned methods of risk assessment step a, when detecting influence of the plastic products migration thing to vinasse, institute
The wine product stated is the distillate that vinasse are added after water distillation;Described analogies are analogies A.
It is preferred that, in above-mentioned methods of risk assessment step a, when detecting influence of the plastic products migration thing to finished wine,
Described wine product is finished wine;Described analogies are at least one of analogies B or analogies C.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the GC-MS are:GC testing conditions are:Rise
Warm program:40 DEG C of holding 5min, are warming up to 220 DEG C of holding 10min, then be warming up to 280 DEG C of holdings with 5 DEG C/min with 4 DEG C/min
5min;Or 40 DEG C of holding 1min, 220 DEG C of holding 1min are warming up to 6 DEG C/min, then 280 DEG C of holdings are warming up to 5 DEG C/min
5min;Sample size:1~5uL;Input mode:Splitless injecting samples.
Further, in above-mentioned methods of risk assessment step b, the testing conditions of the GC-MS are:GC detections are used
Gas chromatographic column is:HPINWAX 60m*0.25mm*0.25 μm or HP-5Agilent30m*0.25mm*0.25 μm.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the GC-MS are:MS testing conditions are:Electricity
From mode:EI;Scan mode:Full scan;Ionizing energy:70ev;Mass scan range:30~550.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the LC-QTOF are:LC testing conditions are:
Mobile phase:Methanol B, ultra-pure water A;Gradient elution:0~12min:10%B~100%B, 12min~20min:100%B,
20min~22min:100%B~10%B, 22min:Stop;Column temperature:20~30 DEG C;Flow velocity:0.1~0.3mL/min;Sample introduction
Volume:1~5uL.
Further, in above-mentioned methods of risk assessment step b, the testing conditions of the LC-QTOF are:LC detections are used
Chromatographic column be:Agilent Eclipse Plus C18 2.1*50mm 1.8-micron.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the LC-QTOF are:QTOF testing conditions
For:Ion gun:DESI sources;The holotype condition of scanning:Dry temperature degree:300℃;Dry gas stream amount:10L/min;Atomizer pressure
Power:40psig;Capillary voltage:4000v;Capillary outlet voltage:60v;The negative mode condition of scanning:Dry temperature degree:300
℃;Dry gas stream amount:8L/min;Nebulizer pressure:40psig;Capillary voltage:3500v;Capillary outlet voltage:60v.
Specifically, in above-mentioned methods of risk assessment step b, the testing conditions of the ICP-MS are:Scan pattern:Sweep entirely
Retouch;Scanning times:100;Forward power:1400W;Residence time:10000μs;Sampling time:13s;Sampling depth:
159step;Cooling gas flow:13.0L/min;Secondary air amount:0.70L/min;Atomization gas flow:0.95L/min;Peristaltic pump
Rotating speed:25r/min;Number of repetition:3.
The determination of test example 1, analogies and simulated conditions
Because service condition of the plastic products in vinasse and finished wine is entirely different, therefore, point vinasse and finished wine are examined
Consider analogies and simulated conditions.
1. the determination of vinasse analogies and simulated conditions
The plastic products used in fermentation process are mainly the slippers that the plastic cloth for taking cellar for storing things and roasting wine workman wear, most wine
The vinasse of factory are not directly contacted with plastic cloth, also have a small number of breweries directly to put up pit with plastic cloth.The slippers that roasting wine workman wears are several
It is that PVC material is done, plasticiser is easily advanced into vinasse, then is brought into wine.
A) determination of vinasse analogies
Liquor production is all solid state fermentation, and the vinasse wine degree of various odor types is about all 5%, and Laobaigan-flavour acidity is most
It is low, about 2%, Luzhou-flavor acidity highest, about 5%, that is to say, that vinasse acidity is between 2~5%.Acidity is higher, dissolution
Material it is more, therefore, we by Luzhou-flavor vinasse acidity setting analogies A, i.e. spirituosity 4~6%, acetic acid 4~6%
The aqueous solution;It is preferred that analogies A is spirituosity 5%, the aqueous solution of acetic acid 5%, 1 is shown in Table.
B) determination of vinasse simulated conditions
The fermentation time of odor type difference vinasse is different, and the vinasse fermentation time of Laobaigan-flavour is most short about 20 days, giving off a strong fragrance
Type fermentation time is most long about 70 days, and interior temperature in cellar is at 30 DEG C or so, with reference to GB/T 23296.1-2009《Food contact material
Material is tested and content assaying method and food to food and food simulants specific transfer in restricted substances plastics in plastics
The guide of analogies exposure condition selection》, set the 10 days migration test time of simulated conditions, 40 ± 1 DEG C of migration test temperature;
It is preferred that the 10 days migration test time of simulated conditions, 40 DEG C of migration test temperature, are shown in Table 2.
Table 1 is used for the analogies for migrating thing measure
Table 2 carries out time and the temperature conditionss of migration test using analogies
The migration test time | 10 days |
Migration test temperature | 40±1℃ |
2. the determination of wine analogies and simulated conditions
The plastic products contacted with finished wine mainly have bottle cap, bottle, envelope altar plastic cloth, wine conveying pipe road, storage container etc.,
It is most straightforward approach that plastic products are directly soaked with wine product, but fragrant liquor is more, and composition is sufficiently complex, wine degree from 25 to
70 degree, one is easy erroneous judgement, and two be the too many trouble of experiment, therefore needs design simulation thing, is used again according to the situation of simulation analyte detection
Finished wine makees last judgement.
A) determination of white wine analogies
It is low that the wine degree for the base liquor that each company produces has height to have, and Maotai-flavor liquor only has spends more 50, and delicate fragrance type wine can reach
Similar 80 degree, but delicate fragrance type vinic acid degree is low, and Maotai-flavor liquor acidity is high, takes into account various odor types, is considered with most exacting terms, if
Determine analogies B and C, be shown in Table 1.
B) determination of white wine simulated conditions
White wine is the food of long-term storage, and winter temperature is low, but summer temperature is high, and temperature is higher in transit sometimes, presses
Sighting target quasi- GB/T 23296.1-2009 10 days migration test times of setting, 40 ± 1 DEG C of migration test temperature is shown in Table 2.
Test example 2
1) confirmatory experiment that GC-MS is detected to volatile organic matter
GC-MS is the situation for fully understanding the volatile organic matter dissolved into leaching liquor using the purpose of full scan, will be treated
Test sample product sample introduction after analogies soak, while detecting immersion testing sample analogies, compares leaching liquor and analogies GC-
MS collection of illustrative plates, finds increased peak or peak area, computer spectrum storehouse (NIST11) retrieval is carried out to it, in conjunction with artificial spectrogram solution
Analysis, confirms its chemical constitution, suspicious compound need to further be confirmed, such as confirms chemical constitution with standard items, determines
Content etc..
The present inventor has prepared 10 representative standard substances to verify the reliability of qualitatively screening result,
Its detection limit under full scan pattern is determined with Agilent GC7890A-MS5975C.
GC-MS testing conditions are as follows:GC testing conditions are:Heating schedule:40 DEG C of holding 5min, are warming up to 4 DEG C/min
220 DEG C of holding 10min, then 280 DEG C of holding 5min are warming up to 5 DEG C/min;Or 40 DEG C of holding 1min, it is warming up to 6 DEG C/min
220 DEG C of holding 1min, then 280 DEG C of holding 5min are warming up to 5 DEG C/min;Sample size:1uL or 2uL;Input mode:Do not shunt
Sample introduction;MS testing conditions are:Ionization mode:EI;Scan mode:Full scan;Ionizing energy:70ev;Mass scan range:30~
550;As a result 3 be see the table below:
The GC-MS detection limits of 3 10 compounds of table
Sequence number | Title | Concentration (mg/L) |
1 | Dibutyl phthalate (DBP) | 0.2 |
2 | Trimethylpyrazine | 0.5 |
3 | Furfural | 0.2 |
4 | P-methyl phenol | 0.2 |
5 | Triethylamine | 2 |
6 | Ethyl palmitate | 1 |
7 | Benzoic acid -2- ethylhexyls | 0.2 |
8 | 2-Ethylhexyl Alcohol | 0.2 |
9 | 4- methyl -2,6 di t butyl phenol | 5 |
10 | Benzothiazole | 1 |
As can be seen from Table 3, the compound detection limit that the detection limit of 10 kinds of materials of the above has in a liter milligram level, table 3
It is higher, such as triethylamine, 4- methyl -2,6- DI-tert-butylphenol compounds, although the GC-MS detection limits of these compounds are higher, but these
The LC-MS detection limits of compound are very low, and along with volatile compound is easily smelt, sense organ can also make up a few compounds
The higher deficiency of GC-MS detection limits.Therefore the volatile organic matter under GC-MS full scan patterns in qualitatively screening plastic products is
Feasible.
2) confirmatory experiment that LC-QTOF is detected to higher-boiling compound
Liquid-matter is adapted under the higher-boiling compound in detection leaching liquor, LC-QTOF holotypes to heterocyclic compound sensitivity
It is very high, it is very high to the sensitivity of organic acid, phenol etc. under negative mode, using LC-QTOF under holotype and negative mode state
Carry out the high boiling point organic compound in full scan, detection leaching liquor.While detecting leaching liquor, detection immersion is to be measured under the same terms
The analogies of sample, compare the LC-MS collection of illustrative plates of leaching liquor and analogies, find the peak or the more peak of abundance increase increased,
Molecular formula is parsed according to mass-to-charge ratio, the element composition of fragment ion is further parsed, utilizes the hands such as artificial parsing and standard specimen
The compound is identified section.
The present inventor is in order to verify the reliability of qualitatively screening result, with Agilent LC1290-QTOF6520B holotypes
With full scan is carried out under negative mode state.
LC-QTOF testing conditions are as follows:LC testing conditions are:Mobile phase:Methanol B, ultra-pure water A;Gradient elution:0~
12min:10%B~100%B, 12min~20min:100%B, 20~22min:100%B~10%B, 22min:stop;Post
Temperature:25℃;Flow velocity:0.2mL/min;Sampling volume:5uL;QTOF testing conditions are:Ion gun:DESI sources;Holotype scan stripes
Part:Dry temperature degree:300℃;Dry gas stream amount:10L/min;Nebulizer pressure:40psig;Capillary voltage:4000v;Hair
Tubule exit potential:60v;The negative mode condition of scanning:Dry temperature degree:300℃;Dry gas stream amount:8L/min;Atomizer pressure
Power:40psig;Capillary voltage:3500v;Capillary outlet voltage:60v.
The detection limit result such as table 4 below of moieties:
The LC-QTOF detection limits of the part of compounds of table 4
As can be seen from Table 4, LC-QTOF detection sensitivity is very high, all in Gamma Magnitude.Generally, national standard is advised
The limitation of poisonous and harmful substance in fixed food is all more than Gamma Magnitude, therefore, and qualitatively screening poisonous and harmful substance is that do not have
Problem.
3) confirmatory experiments of the ICP-MS to metal ion detection
ICP-MS full scans, which are mainly, detects that plastic products move to the organic matter containing metallic element in analogies, with
Gas-matter, liquid-matter are identical, detect analogies while detection leaching liquor, compare the ICP-MS spectrograms of leaching liquor and analogies, very
Easily find increased metallic element.
Inventor is in order to verify the reliability of qualitatively screening result, with Themore companies of U.S. X-series2 inductives
The detection limit of the metal ion of plasma mass spectrograph.
ICP-MS testing conditions:Scan pattern:Full scan;Scanning times:100;Forward power:1400W;Residence time:
10000μs;Sampling time:13s;Sampling depth:159step;Cooling gas flow:13.0L/min;Secondary air amount:0.70L/
min;Atomization gas flow:0.95L/min;Wriggling revolution speed:25r/min;Number of repetition:3.
As a result such as table 5 below:
The ICP-MS detection limits of the main metal element of table 5
As can be seen from Table 5, Inductively coupled plasma mass spectrometry is very high to the detection sensitivity of metallic element, all exists
Winged gram is arrived Gamma Magnitude, is without a doubt with compound of the ICP-MS qualitatively screenings containing metallic element therefore.
4) organoleptic detection
For aroma compound, the sensory acuity of people is usually above instrument and equipment, therefore judges plastics with organoleptic detection
Product migrates influence of the thing to vinosity.
Experienced personnel 5-7 people composition of tasting and appraising tastes and appraise group, organoleptic detection plastic products, leaching liquor and control sample, wine
Too high influence the as needed of organoleptic detection of smart concentration is quantitatively diluted.The evaluation influenceed on sample organoleptic feature, is referred to
The comment that organoleptic requirements part is provided in Liquor Products standard, expresses poor with reference to the degree adverb such as " slight ", " compared with ", " protrusion "
Not.Such as need, to sense organ quantitative descriptive analysis, to use《GB 12313-1990 sensory testing methods local flavors section is examined》Method is combined
Liquor flavor parameter, to product sensory feature and intensity or persistence quantitative expression.
Embodiment 1, with the inventive method assess pvc pipe as wine conveying pipe road security
By simulating analyte detection:Pvc pipe is cut into individual particle≤0.02g fine particle, is well mixed, accurately weighs
5g samples (being accurate to 0.1mg) are separately added into 50mL analogies B, 50mL analogies C, are put into 40 DEG C ± 1 in conical flask with stopper
DEG C insulating box in, take leaching liquor to detect after daily shaking flask 1-2 times, 10 days.
Verified and detected by wine sample:Ibid after processing PVC, accurately weigh 5g samples (being accurate to 0.1mg) and fill in triangle in tool
In bottle, it is separately added into 68 ° of Luzhou-flavor base liquors of 50mL, 53 ° of Maotai-flavors and 59 ° of delicate fragrance type wine, is put into 40 DEG C ± 1 DEG C of perseverance
In incubator, leaching liquor is taken to detect after daily shaking flask 1-2 times, 10 days.
Testing conditions:
1), GC-MS conditions are:GC testing conditions are:Heating schedule:40 DEG C of holding 5min, 220 are warming up to 4 DEG C/min
DEG C keep 10min, then with 5 DEG C/min be warming up to 280 DEG C holding 5min;Or 40 DEG C of holding 1min, it is warming up to 220 with 6 DEG C/min
DEG C keep 1min, then with 5 DEG C/min be warming up to 280 DEG C holding 5min;Sample size:1uL or 2uL;Input mode:It is not diverted into
Sample;MS testing conditions are:Ionization mode:EI;Scan mode:Full scan;Ionizing energy:70ev;Mass scan range:30~
550。
2), LC-QTOF testing conditions:LC testing conditions are:Mobile phase:Methanol B, ultra-pure water A;Gradient elution:0~
12min:10%B~100%B, 12min~20min:100%B, 20~22min:100%B~10%B, 22min:stop;Post
Temperature:25℃;Flow velocity:0.2mL/min;Sampling volume:5uL;QTOF testing conditions are:Ion gun:DESI sources;Holotype scan stripes
Part:Dry temperature degree:300℃;Dry gas stream amount:10L/min;Nebulizer pressure:40psig;Capillary voltage:4000v;Hair
Tubule exit potential:60v;The negative mode condition of scanning:Dry temperature degree:300℃;Dry gas stream amount:8L/min;Atomizer pressure
Power:40psig;Capillary voltage:3500v;Capillary outlet voltage:60v.
3), ICP-MS testing conditions:Scan pattern:Full scan;Scanning times:100;Forward power:1400W;When resident
Between:10000μs;Sampling time:13s;Sampling depth:159step;Cooling gas flow:13.0L/min;Secondary air amount:
0.70L/min;Atomization gas flow:0.95L/min;Wriggling revolution speed:25r/min;Number of repetition:3.
Luzhou-flavor base liquor five-Grain Liquor base liquor in the present embodiment, Maotai-flavor liquor Maotai, delicate fragrance type wine Fenyang wine.
1) GC-MS spectrograms are shown in Fig. 1-10, as a result show:
A, a, when being verified using Luzhou-flavor base liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies B makees
For blank sample and the spectrogram difference of the leaching liquor of gained, both are close at difference;
B, when being verified using Maotai-flavor liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies B is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
C, when being verified using delicate fragrance type wine the leaching liquor of blank sample and gained spectrogram difference, and analogies B is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies B can truly reflect
Go out the moving in the finished wine of the different wine degree of major odor types such as Luzhou-flavor, delicate fragrance type, Maotai-flavor of the migration thing in plastic products
Shift one's love condition;Meanwhile, migrate thing dissolution situation in white wine and analogies by plastic products and be combineding with each other and verify, more can be accurate
Really judge that plastic products are used for the security of wine product.
B, a, when being verified using Luzhou-flavor base liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies C makees
For blank sample and the spectrogram difference of the leaching liquor of gained, both are close at difference;
B, when being verified using Maotai-flavor liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies C is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
C, when being verified using delicate fragrance type wine the leaching liquor of blank sample and gained spectrogram difference, and analogies C is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies C can truly reflect
Go out the moving in the finished wine of the different wine degree of major odor types such as Luzhou-flavor, delicate fragrance type, Maotai-flavor of the migration thing in plastic products
Shift one's love condition;Meanwhile, migrate thing dissolution situation in white wine and analogies by plastic products and be combineding with each other and verify, more can be accurate
Really judge that plastic products are used for the security of wine product.
2) LC-QTOF spectrograms are shown in Figure 11-20, as a result show:
A, a, when being verified using Luzhou-flavor base liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies B makees
For blank sample and the spectrogram difference of the leaching liquor of gained, both are close at difference;
B, when being verified using Maotai-flavor liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies B is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
C, when being verified using delicate fragrance type wine the leaching liquor of blank sample and gained spectrogram difference, and analogies B is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies B can truly reflect
Go out the moving in the finished wine of the different wine degree of major odor types such as Luzhou-flavor, delicate fragrance type, Maotai-flavor of the migration thing in plastic products
Shift one's love condition;Meanwhile, migrate thing dissolution situation in white wine and analogies by plastic products and be combineding with each other and verify, more can be accurate
Really judge that plastic products are used for the security of wine product.
B, a, when being verified using Luzhou-flavor base liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies C makees
For blank sample and the spectrogram difference of the leaching liquor of gained, both are close at difference;
B, when being verified using Maotai-flavor liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies C is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
C, when being verified using delicate fragrance type wine the leaching liquor of blank sample and gained spectrogram difference, and analogies C is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies C can truly reflect
Go out the moving in the finished wine of the different wine degree of major odor types such as Luzhou-flavor, delicate fragrance type, Maotai-flavor of the migration thing in plastic products
Shift one's love condition;Meanwhile, migrate thing dissolution situation in white wine and analogies by plastic products and be combineding with each other and verify, more can be accurate
Really judge that plastic products are used for the security of wine product.
3) ICP-MS spectrograms are shown in Figure 21-30, as a result show:
A, a, when being verified using Luzhou-flavor base liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies B makees
For blank sample and the spectrogram difference of the leaching liquor of gained, both are close at difference;
B, when being verified using Maotai-flavor liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies B is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
C, when being verified using delicate fragrance type wine the leaching liquor of blank sample and gained spectrogram difference, and analogies B is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies B can truly reflect
Go out the moving in the finished wine of the different wine degree of major odor types such as Luzhou-flavor, delicate fragrance type, Maotai-flavor of the migration thing in plastic products
Shift one's love condition;Meanwhile, migrate thing dissolution situation in white wine and analogies by plastic products and be combineding with each other and verify, more can be accurate
Really judge that plastic products are used for the security of wine product.
B, a, when being verified using Luzhou-flavor base liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies C makees
For blank sample and the spectrogram difference of the leaching liquor of gained, both are close at difference;
B, when being verified using Maotai-flavor liquor the leaching liquor of blank sample and gained spectrogram difference, and analogies C is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
C, when being verified using delicate fragrance type wine the leaching liquor of blank sample and gained spectrogram difference, and analogies C is used as blank
The spectrogram difference of the leaching liquor of sample and gained, both are close at difference;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies C can truly reflect
Go out the moving in the finished wine of the different wine degree of major odor types such as Luzhou-flavor, delicate fragrance type, Maotai-flavor of the migration thing in plastic products
Shift one's love condition;Meanwhile, migrate thing dissolution situation in white wine and analogies by plastic products and be combineding with each other and verify, more can be accurate
Really judge that plastic products are used for the security of wine product.
For analogies B and C selection, analogies C wine degree is higher than analogies B, and the migration thing of plastic products is also more,
If requirement of the enterprise to finished wine is higher, analogies C can be used, requirement can be met when using analogies C, then adopt
With analogies B necessarily satisfying for requiring;If requirement of the enterprise to finished wine is slightly lower, using analogies B just, then specifically adopt
All used, can voluntarily be selected according to the requirement of enterprise with any analogies or both.
Organoleptic detection result
To sum up, from Fig. 1-2 0 as can be seen that the white wine and the GC-MS of its corresponding soak of each odor type, LC-QTOF,
After ICP-MS contrasts, the spectrogram overwhelming majority before and after immersion is all changed;The GC-MS of analogies soak corresponding with its,
After LC-QTOF, ICP-MS contrast, the spectrogram overwhelming majority before and after immersion is all changed;Both change basically identical, so,
First:The migration situation of compound when analogies B and analogies C can reflect different white wine contact plastic products, and it is more straight
See, be more easy to analysis and judge, therefore, it is feasible that analogies B and analogies C, which are used as white wine analogies,;Second:Pass through plastic products
Migrate thing dissolution situation in white wine and analogies be combineding with each other and verifying, more can judge that plastic products are used for wine production exactly
The security of product.
So, either individually from the point of view of dissolution situation of the plastic products in analogies, or by plastic products white
From the point of view of dissolution situation in wine and analogies is combined, the result of the present embodiment illustrates that the pvc pipe is used as white wine wine conveying pipe road
There is food safety risk.
Embodiment 2, safety and quality risk with the inventive method assessment PE envelope cellar for storing things plastic clothes
By simulating analyte detection:PE plastic clothes are shredded into less than 0.5cm2Fragment, be well mixed, in 10% ratio
The sample prepared is put into analogies A, places ten days, shakes up 1-2 times daily in 40 DEG C of insulating boxs.
Verified and detected by vinasse:Place length and width 50cm plastic clothes to put up after vinasse again with pit sealing mud envelope cellar for storing things, ferment within 70 days
Detection contacts the sense organ and physical and chemical index of vinasse with plastic cloth after phase terminates, and the vinasse ratio of plastic cloth is not put up with same position
Compared with.Vinasse thick 5cm under PE plastic clothes are taken, 100g vinasse add 100mL water to distill, and take distillate 5mL to detect;Comparative example, which takes, not to be had
Put up the vinasse of the same position of plastic cloth.
Testing conditions:
1), GC-MS conditions are:GC testing conditions are:Heating schedule:40 DEG C of holding 5min, 220 are warming up to 4 DEG C/min
DEG C keep 10min, then with 5 DEG C/min be warming up to 280 DEG C holding 5min;Or 40 DEG C of holding 1min, it is warming up to 220 with 6 DEG C/min
DEG C keep 1min, then with 5 DEG C/min be warming up to 280 DEG C holding 5min;Sample size:1uL or 2uL;Input mode:It is not diverted into
Sample;MS testing conditions are:Ionization mode:EI;Scan mode:Full scan;Ionizing energy:70ev;Mass scan range:30~
550。
2), LC-QTOF testing conditions:LC testing conditions are:Mobile phase:Methanol B, ultra-pure water A;Gradient elution:0~
12min:10%B~100%B, 12min~20min:100%B, 20~22min:100%B~10%B, 22min:stop;Post
Temperature:25℃;Flow velocity:0.2mL/min;Sampling volume:5uL;QTOF testing conditions are:Ion gun:DESI sources;Holotype scan stripes
Part:Dry temperature degree:300℃;Dry gas stream amount:10L/min;Nebulizer pressure:40psig;Capillary voltage:4000v;Hair
Tubule exit potential:60v;The negative mode condition of scanning:Dry temperature degree:300℃;Dry gas stream amount:8L/min;Atomizer pressure
Power:40psig;Capillary voltage:3500v;Capillary outlet voltage:60v.
3), ICP-MS testing conditions:Scan pattern:Full scan;Scanning times:100;Forward power:1400W;When resident
Between:10000μs;Sampling time:13s;Sampling depth:159step;Cooling gas flow:13.0L/min;Secondary air amount:
0.70L/min;Atomization gas flow:0.95L/min;Wriggling revolution speed:25r/min;Number of repetition:3.
1) GC-MS spectrograms are shown in Figure 31-34, as a result show:
When using vinasse verify when blank sample (vinasse add water distillation after distillate) and gained leaching liquor spectrogram
Difference results, and analogies A are close with the spectrogram difference results of the leaching liquor of gained as blank sample;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies A can truly reflect
Migration situation of the migration thing in vinasse gone out in plastic products;Meanwhile, thing is migrated in vinasse and analogies by plastic products
Be combineding with each other and verifying for middle dissolution situation, can more judge that plastic products are used for the security of wine product exactly.
2) LC-QTOF spectrograms are shown in Figure 35-38, as a result show:
When using vinasse verify when blank sample (vinasse add water distillation after distillate) and gained leaching liquor spectrogram
Difference results, and analogies A are close with the spectrogram difference results of the leaching liquor of gained as blank sample;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies A can truly reflect
Migration situation of the migration thing in vinasse gone out in plastic products;Meanwhile, thing is migrated in vinasse and analogies by plastic products
Be combineding with each other and verifying for middle dissolution situation, can more judge that plastic products are used for the security of wine product exactly.
3) ICP-MS spectrograms are shown in Figure 39-42, as a result show:
When using vinasse verify when blank sample (vinasse add water distillation after distillate) and gained leaching liquor spectrogram
Difference results, and analogies A are close with the spectrogram difference results of the leaching liquor of gained as blank sample;
It in summary it can be seen, migration situation of the plastic products in the inventive method in analogies A can truly reflect
Migration situation of the migration thing in vinasse gone out in plastic products;Meanwhile, thing is migrated in vinasse and analogies by plastic products
Be combineding with each other and verifying for middle dissolution situation, can more judge that plastic products are used for the security of wine product exactly.
Sensory results:
To sum up, from Figure 21-42 as can be seen that GC-MS, LC-QTOF, ICP-MS couple of vinasse and its corresponding soak
Than after, the spectrogram before and after immersion is substantially without change;GC-MS, LC-QTOF, ICP-MS couple of analogies soak corresponding with its
Than after, the spectrogram before and after immersion is substantially without change;So, first:Analogies A can reflect chemical combination when vinasse contact plastic products
The migration situation of thing, and the time is short, it is easy to and analysis judges that therefore, it is feasible that analogies A, which is used as vinasse analogies,;Second:
Thing dissolution situation in vinasse and analogies is migrated by plastic products to be combined with each other and verifying, can more judge plastics exactly
Product is used for the security of wine product.
So, either individually from the point of view of dissolution situation of the plastic products in analogies, or by plastic products in wine
From the point of view of dissolution situation in grain and analogies is combined, the result of the present embodiment illustrates that the PE plastic clothes are used to put up vinasse to be
There is no food safety risk.
Claims (7)
1. wine brewing production migrates the methods of risk assessment that thing influences on wine product with plastic products, it is characterised in that:Including following
Step:
A, plastic products are crushed after be added in treatment fluid, place under simulated conditions extract, filtering, obtain filtrate, as soak
Extract;Described treatment fluid is any one in wine product or analogies;
B, with GC-MS, LC-QTOF, ICP-MS leaching liquor and treatment fluid are detected respectively, pass through leaching liquor and the spectrogram pair for the treatment of fluid
Than, it was therefore concluded that;
The testing conditions of the GC-MS are:GC testing conditions are:Heating schedule:40 DEG C of holding 5min, are warming up to 4 DEG C/min
220 DEG C of holding 10min, then 280 DEG C of holding 5min are warming up to 5 DEG C/min;Or 40 DEG C of holding 1min, it is warming up to 6 DEG C/min
220 DEG C of holding 1min, then 280 DEG C of holding 5min are warming up to 5 DEG C/min;Sample size:1~5uL;Input mode:It is not diverted into
Sample;MS testing conditions are:Ionization mode:EI;Scan mode:Full scan;Ionizing energy:70ev;Mass scan range:30~
550;
The testing conditions of the LC-QTOF are:LC testing conditions are:Mobile phase:Methanol B, ultra-pure water A;Gradient elution:0~
12min:10%B~100%B, 12min~20min:100%B, 20min~22min:100%B~10%B, 22min:Stop
Only;Column temperature:20~30 DEG C;Flow velocity:0.1~0.3mL/min;Sampling volume:1~5uL;QTOF testing conditions are:Ion gun:
DESI sources;The holotype condition of scanning:Dry temperature degree:300℃;Dry gas stream amount:10L/min;Nebulizer pressure:40psig;
Capillary voltage:4000v;Capillary outlet voltage:60v;The negative mode condition of scanning:Dry temperature degree:300℃;Dry gas stream
Amount:8L/min;Nebulizer pressure:40psig;Capillary voltage:3500v;Capillary outlet voltage:60v;
The testing conditions of the ICP-MS are:Scan pattern:Full scan;Scanning times:100;Forward power:1400W;When resident
Between:10000μs;Sampling time:13s;Sampling depth:159step;Cooling gas flow:13.0L/min;Secondary air amount:
0.70L/min;Atomization gas flow:0.95L/min;Wriggling revolution speed:25r/min;Number of repetition:3.
2. wine brewing production according to claim 1 migrates the methods of risk assessment that thing influences on wine product with plastic products,
It is characterized in that:In step a, described simulated conditions are 40 DEG C ± 1 DEG C of soaking temperature, soak time 10d.
3. wine brewing production according to claim 1 migrates the methods of risk assessment that thing influences on wine product with plastic products,
It is characterized in that:In step a, described analogies are analogies A, spirituosity 4~6%, the aqueous solution of acetic acid 4~6%.
4. wine brewing production according to claim 1 migrates the methods of risk assessment that thing influences on wine product with plastic products,
It is characterized in that:In step a, described analogies are analogies B, spirituosity 50~70%, the aqueous solution of acetic acid 0.5~1%.
5. wine brewing production according to claim 1 migrates the methods of risk assessment that thing influences on wine product with plastic products,
It is characterized in that:In step a, described analogies are analogies C, containing 90~100% alcohol.
6. wine brewing production according to claim 1 migrates the methods of risk assessment that thing influences on wine product with plastic products,
It is characterized in that:In step a, when detecting influence of the plastic products migration thing to vinasse, described wine product adds for vinasse
Distillate after water distillation;Described analogies are spirituosity 4~6%, the aqueous solution of acetic acid 4~6%.
7. wine brewing production according to claim 1 migrates the methods of risk assessment that thing influences on wine product with plastic products,
It is characterized in that:In step a, when detecting influence of the plastic products migration thing to wine, described wine product is finished wine;It is described
Analogies be spirituosity 50~70%, the aqueous solution of acetic acid 0.5~1% or containing at least one of 90~100% alcohol.
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