CN107064371A - The detection method of multiple harmful substances in a kind of fast food wrappers bag - Google Patents
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- CN107064371A CN107064371A CN201710290848.6A CN201710290848A CN107064371A CN 107064371 A CN107064371 A CN 107064371A CN 201710290848 A CN201710290848 A CN 201710290848A CN 107064371 A CN107064371 A CN 107064371A
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- 239000000126 substance Substances 0.000 title claims abstract description 32
- 235000013410 fast food Nutrition 0.000 title claims abstract description 26
- 238000001514 detection method Methods 0.000 title claims abstract description 24
- 238000002386 leaching Methods 0.000 claims abstract description 72
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 238000005374 membrane filtration Methods 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000004817 gas chromatography Methods 0.000 claims abstract description 4
- 238000007654 immersion Methods 0.000 claims abstract description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 63
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 38
- 238000010792 warming Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012634 fragment Substances 0.000 claims description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 235000013305 food Nutrition 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 4
- 239000005416 organic matter Substances 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 238000002347 injection Methods 0.000 description 9
- 239000007924 injection Substances 0.000 description 9
- 239000012159 carrier gas Substances 0.000 description 6
- 238000001819 mass spectrum Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000004519 grease Substances 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004949 mass spectrometry Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004451 qualitative analysis Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 235000013194 Lyophyllum decastes Nutrition 0.000 description 1
- 240000005856 Lyophyllum decastes Species 0.000 description 1
- 241000124033 Salix Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 235000012771 pancakes Nutrition 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
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
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The detection method of multiple harmful substances, specifically includes following steps in a kind of fast food wrappers bag of the present invention：Step 1, paper bag to be measured is shredded, obtains shredded paper bits；Step 2, the shredded paper bits obtained by step 1 are soaked in soak, then immersion 0.5h~1.5h leaches and extract leaching liquid；Step 3, the leaching liquid that step 2 is extracted is evaporated concentration, by the leaching liquid after concentration through organic membrane filtration；Step 4, the leaching liquid after the filtering obtained by step 3 is tested by gas chromatography mass spectrometer, is that can determine that the harmful substance in paper bag according to test result.The detection method of multiple harmful substances is compared with conventional single detection method in a kind of fast food wrappers bag proposed by the present invention, it is simple, convenient and rapid, economically feasible, the variety classes harmful substance suitable for film fast food paper bag is while qualitative detection, is that the quantitative detection of organic matter in food contact material is laid a good foundation.
Description
Technical field
The invention belongs to wrapping paper detection technique field, it is related to multiple harmful substances in a kind of fast food wrappers bag
Detection method.
Background technology
As the improvement of people's living standards, food-safety problem receives extensive concern.Packaging for foodstuff be in food not
Whether the part that can or lack, food packaging safety can have influence on food security to a great extent.
The packaging for foodstuff of the fast food in the market overwhelming majority is papery packaging, and the basis of paper wrapper is to plant
Fibres, can add a large amount of auxiliary agents in process of production, and packaging and food can be contacted in some cases, now in external environment
Under the influence of (temperature, humidity etc.), some harmful substances can be progressed into food, so as to be caused harm to health.
Contain many harmful substances in the printing-ink of papery packaging, and be present some defects in printing paper surface, hold
Paper surface dissolvent residual is easily caused, these solvents are likely to move to food during food wrapper use, right
Human health produces potential threat；Also some volatile organic matters, they are also potentially harmful substance in food wrapper,
Human health and environmental quality can be influenceed by being discharged into environment.
As China industrializes, urbanization and modernization are accelerated increasingly, fast food rapid growth, the market share is continuous
Expand, occupied the share of catering market 45 about percent, food wrapper demand is also increased substantially.Disposably
Paper bag, carton are largely used to fast food packaging, adapt to popular work and accelerate with rhythm of life.According to correlative study in dining process
In the harmful organic substance that contains in food packaging paper naturally can infiltration migration eaten in vivo into food, and then by consumer,
So as to endanger the healthy of people.Dissolvent residual is badly in need of paying attention in fast food packaging material, is harmful in food wrapper
Content of material must be controlled in comparatively safe scope, it is therefore necessary to which the harmful substance remained in packaging material for food is entered
Row detection.But conventional detection method is to detect the single harmful substance in food wrapper, detection efficiency is relatively low, unfavorable
The safe coefficient of food wrapper is evaluated in comprehensive analysis, being badly in need of variety classes a kind of bag suitable for fast food wrappers has
Evil material is while the method for qualitative detection.
The content of the invention
It is an object of the invention to provide a kind of fast food wrappers bag in multiple harmful substances detection method, for pair
Harmful substance in packaging for foodstuff paper bag is detected.
The technical solution adopted in the present invention is, the detection side of multiple harmful substances in a kind of fast food wrappers bag
Method, specifically includes following steps：
Step 1, paper bag to be measured is shredded, obtains shredded paper bits；
Step 2, the shredded paper bits obtained by step 1 are soaked in soak, immersion 0.5h -1.5h and then leaching are simultaneously
Extract leaching liquid；
Step 3, the leaching liquid that step 2 is extracted is evaporated concentration, by the leaching liquid after concentration through organic membrane filtration；
Step 4, the leaching liquid after the filtering obtained by step 3 is tested by gas chromatography mass spectrometer, according to test
As a result it can determine that the harmful substance in paper bag.
The features of the present invention is also resided in,
Shredded paper bits wherein obtained by step 1 are square fragment.
Soak wherein in step 2 is n-hexane and the mixed liquor of dichloromethane, and n-hexane and dichloromethane with 1~
2:1 volume ratio mixing.
Leaching wherein in step 2 is supersonic leaching, during supersonic leaching the supersonic frequency of ultrasonic generator be 20~
40kHz, ultrasonic power is 120~300W, and the temperature of supersonic leaching is 30~40 DEG C, and the supersonic leaching time is 15~30min, is surpassed
Sound leaching cycle number of times is 2~3 times.
The detailed process of wherein step 3 is as follows：
The leaching liquid that step 2 is extracted is transferred in rotary evaporation bottle, and rotary evaporation is used under 30~40 DEG C of water bath conditions
Instrument is concentrated, and the leaching liquid volume after concentration is 1/10th of leaching liquid volume before concentration, and the leaching liquid after concentration is shaken into equal
Through 0.22 μm of organic membrane filtration after even.
The initial temperature of temperature-rise period wherein in step 4 in gas chromatography-mass spectrometry work is 30~50 DEG C, is protected
2~5min is held, then 170~190 DEG C are warming up to 5~10 DEG C/min speed, then be warming up to 3~5 DEG C/min speed
250~270 DEG C, keep 20~25min, finally using Splitless injecting samples, sample size be 1 μ L, the solvent delay time be 8~
15min。
The beneficial effects of the invention are as follows the inspection of multiple harmful substances in a kind of fast food wrappers bag proposed by the present invention
Survey method is compared with conventional single determination method, simple, convenient and rapid, economically feasible, it is adaptable to different in film fast food paper bag
Species harmful substance is while qualitative detection, is that the quantitative detection of organic matter in food contact material is laid a good foundation, is further
The migration for studying harmful substance in food wrapper provides foundation.
Embodiment
With reference to embodiment, the present invention is described in detail.
The detection method of multiple harmful substances in a kind of fast food wrappers bag of the present invention, detailed process is as follows：
Step 1, paper bag to be measured is shredded, obtains shredded paper bits；
Shredded paper bits obtained by step 1 are square fragment.
Step 2, the shredded paper bits obtained by step 1 are soaked in soak, immersion 0.5h -1.5h and then leaching are simultaneously
Extract leaching liquid；
Soak in step 2 is n-hexane and the mixed liquor of dichloromethane, and n-hexane and dichloromethane are with 1~2:1
Volume ratio mixing.
Leaching in step 2 is supersonic leaching, and the supersonic frequency of ultrasonic generator is 20~40kHz during supersonic leaching,
Ultrasonic power is 120~300W, and the temperature of supersonic leaching is 30~40 DEG C, and the supersonic leaching time is 15~30min, leaching cycle
Number of times is 2~3 times.
Step 3, the leaching liquid that step 2 is extracted is evaporated concentration, by the leaching liquid after concentration through organic membrane filtration；
The detailed process of step 3 is as follows：
The leaching liquid that step 2 is extracted is transferred in rotary evaporation bottle, and rotary evaporation is used under 30~40 DEG C of water bath conditions
Instrument is concentrated, and the leaching liquid volume after concentration is 1/10th of leaching liquid volume before concentration, and the leaching liquid after concentration is shaken into equal
Through 0.22 μm of organic membrane filtration after even.
Step 4, the leaching liquid after the filtering obtained by step 3 is tested by gas chromatography mass spectrometer, according to test
As a result it can determine that the harmful substance in paper bag.
The initial temperature of temperature-rise period in step 4 in gas chromatography-mass spectrometry work is 30~50 DEG C, holding 2~
5min, is then warming up to 170~190 DEG C with 5~10 DEG C/min speed, then 250 are warming up to 3~5 DEG C/min speed~
270 DEG C, 20~25min is kept, finally using Splitless injecting samples, sample size is 1 μ L, and the solvent delay time is 8~15min.
It is the printing fast food packaging paper bag for having film to select coated paper envelope to be detected.
Embodiment 1：
The grease proofing paper bag of fried chicken willow in market is purchased from, paper scrap that size is about 3mm*3mm is switched to and is well mixed, weighed
1g is put into 25mL test tubes, and adding the mixed liquor of 10mL n-hexanes and dichloromethane, (volume ratio of n-hexane and dichloromethane is
1:1) 0.5h, is soaked at room temperature first；Secondly it is 40kHz in the supersonic frequency of ultrasonic generator by paper liquid mixture, surpasses
Acoustical power is 240W, and ultrasonic temperature is supersonic leaching 15min under the conditions of 30 DEG C；Leaching liquid is poured out again, 10mL is rejoined
(volume ratio of n-hexane and dichloromethane is 1 to the mixed liquor of n-hexane and dichloromethane:1), in the ultrasound of ultrasonic generator
Frequency is 40kHz, and ultrasonic power is 240W, and ultrasonic temperature is supersonic leaching 15min under the conditions of 30 DEG C；Then leaching liquid is fallen again
Go out, rejoining 10mL n-hexanes and dichloromethane, (n-hexane and methylene chloride volume ratio are 1:1), in ultrasonic generator
Supersonic frequency is 40kHz, and ultrasonic power is 240W, and ultrasonic temperature is supersonic leaching 15min under the conditions of 30 DEG C；Finally by three institutes
The extract solution obtained merges.Room temperature is cooled to after the completion of leaching, leaching liquid is transferred in rotary evaporation bottle, in 30 DEG C of water bath conditions
It is lower to be concentrated into 3mL with Rotary Evaporators, after leaching liquid is shaken uniformly through 0.22 μm of organic membrane filtration into sample injection bottle.In gas
Heating schedule is set on phase chromatograph-mas spectrometer as follows：Initial temperature be 40 DEG C, under the conditions of keep 3.5min, with 8 DEG C/min
Speed be warming up to 180 DEG C, be warming up to 260 DEG C with 4 DEG C/min speed, keep 25min.Splitless injecting samples, the μ L of sample size 1,
Solvent delay 10min.
Chromatographic condition：HP-INNOWAX (60m*0.250mm*0.25 μm) chromatographic column.Injector temperature：250℃；Carrier gas：
He gas；Carrier gas flux：1mL/min.Mass Spectrometry Conditions：Standard mass spectrum is tuned；EI ion guns：Electron energy 70eV；Ion source temperature：
230℃.Level Four bar temperature：150℃；Auxiliary region temperature：30℃.The sample injection bottle for filling leaching liquid is placed on gas chromatography-mass spectrum
In the auto injection mouthful of combined instrument, start is detected；By the document in the calculated value of testing result and NIST14.0 databases
Value compares, to the harmful substance qualitative analysis in fast food wrappers, and result of implementation is organic to detected perfluor in sample
Thing, alkane, benzene homologues.
Embodiment 2：
The grease proofing paper bag of brown paper thin pancake in market is purchased from, paper scrap that size is about 5mm*5mm is switched to and is well mixed,
Weigh 1g to be put into 25mL test tubes, (n-hexane and methylene chloride volume ratio are 2 for addition 15mL n-hexanes and dichloromethane:1) it is, first
First 1h is soaked at room temperature；Secondly it is 30kHz in the supersonic frequency of ultrasonic generator by paper liquid mixture, ultrasonic power is
300W, ultrasonic temperature is supersonic leaching 25min under the conditions of 35 DEG C；Leaching liquid is poured out again, rejoin 15mL n-hexanes and
(n-hexane and methylene chloride volume ratio are 2 to dichloromethane:1) it is, 30kHz, ultrasonic work(in the supersonic frequency of ultrasonic generator
Rate is 300W, and ultrasonic temperature is supersonic leaching 25min under the conditions of 35 DEG C；Finally the extract solution of gained twice is merged.Leach
Room temperature is cooled to after, leaching liquid is transferred in rotary evaporation bottle, is concentrated under 35 DEG C of water bath conditions with Rotary Evaporators
4.5mL, after leaching liquid is shaken uniformly through 0.22 μm of organic membrane filtration into sample injection bottle.In gas chromatograph-mass spectrometer (GC-MS)
Upper setting heating schedule is as follows：Initial temperature be 30 DEG C, under the conditions of keep 2min, be warming up to 170 DEG C with 5 DEG C/min speed,
250 DEG C are warming up to 5 DEG C/min speed, 25min is kept.Splitless injecting samples, sample size 1 μ L, solvent delay 8min.
Chromatographic condition：HP-INNOWAX (60m*0.250mm*0.25 μm) chromatographic column.Injector temperature：250℃；Carrier gas：
He gas；Carrier gas flux：1mL/min.Mass Spectrometry Conditions：Standard mass spectrum is tuned；EI ion guns：Electron energy 70eV；Ion source temperature：
230℃.Level Four bar temperature：150℃；Auxiliary region temperature：30℃.The sample injection bottle for filling leaching liquid is placed on gas chromatography-mass spectrum
In the auto injection mouthful of combined instrument, start is detected；By the document in the calculated value of testing result and NIST14.0 databases
Value compares, to the harmful substance qualitative analysis in fast food wrappers, and result of implementation is organic to detected perfluor in sample
Thing, alkane, benzene homologues.
Embodiment 3：
The grease proofing paper bag of blank sheet of paper pie in market is purchased from, fragment that size is about 2mm*2mm is switched to and is well mixed, is claimed
1g is taken to be put into 25mL test tubes, (n-hexane and methylene chloride volume ratio are 1.5 for addition 10mL n-hexanes and dichloromethane:1) soak
1.5h is steeped, is secondly 20kHz in the supersonic frequency of ultrasonic generator by paper liquid mixture, ultrasonic power is 120W, ultrasound temperature
Spend for supersonic leaching 30min under the conditions of 40 DEG C；Leaching liquid is poured out again, 10mL n-hexanes and dichloromethane is being rejoined (just
Hexane and methylene chloride volume ratio are 1.5:1) it is, 20kHz in the supersonic frequency of ultrasonic generator, ultrasonic power is 120W,
Ultrasonic temperature is supersonic leaching 30min under the conditions of 40 DEG C；Then leaching liquid is poured out again, rejoins 10mL n-hexanes and dichloro
(n-hexane and methylene chloride volume ratio are 1.5 to methane:1) it is, 20kHz, ultrasonic power in the supersonic frequency of ultrasonic generator
For 120W, ultrasonic temperature is supersonic leaching 30min under the conditions of 40 DEG C；Finally the extract solution of three gained is merged.Leaching is completed
After be cooled to room temperature, by leaching liquid be transferred to rotary evaporation bottle in, be concentrated under 40 DEG C of water bath conditions with Rotary Evaporators
3mL, after leaching liquid is shaken uniformly through 0.22 μm of organic membrane filtration into sample injection bottle.On gas chromatograph-mass spectrometer (GC-MS)
Set heating schedule as follows：Initial temperature be 50 DEG C, keep 5min, be warming up to 190 DEG C with 10 DEG C/min speed, with 3 DEG C/
Min speed is warming up to 270 DEG C, keeps 20min.Splitless injecting samples, sample size 1 μ L, solvent delay 15min.
Chromatographic condition：HP-INNOWAX (60m*0.25mm*0.25 μm) chromatographic column.Injector temperature：250℃；Carrier gas：He
Gas；Carrier gas flux：1mL/min.Mass Spectrometry Conditions：Standard mass spectrum is tuned；EI ion guns：Electron energy 70eV；Ion source temperature：
230℃.Level Four bar temperature：150℃；Auxiliary region temperature：30℃.The sample injection bottle for filling leaching liquid is placed on gas chromatography-mass spectrum
In the auto injection mouthful of combined instrument, start is detected；By the document in the calculated value of testing result and NIST14.0 databases
Value compares, to the harmful substance qualitative analysis in fast food wrappers.Result of implementation is organic to detected perfluor in sample
Thing, alkane, benzene homologues.
Claims (6)
1. the detection method of multiple harmful substances in a kind of fast food wrappers bag, it is characterised in that：Specifically include following step
Suddenly：
Step 1, paper bag to be measured is shredded, obtains shredded paper bits；
Step 2, the shredded paper bits obtained by step 1 are soaked in soak, then immersion 0.5h -1.5h leaches and extract
Leaching liquid；
Step 3, the leaching liquid that step 2 is extracted is evaporated concentration, by the leaching liquid after concentration through organic membrane filtration；
Step 4, the leaching liquid after the filtering obtained by step 3 is tested by gas chromatography mass spectrometer, according to test result
It can determine that the harmful substance in paper bag.
2. the detection method of multiple harmful substances, its feature in a kind of fast food wrappers bag according to claim 1
It is：Shredded paper bits obtained by the step 1 are square fragment.
3. the detection method of multiple harmful substances, its feature in a kind of fast food wrappers bag according to claim 1
It is：Soak in the step 2 is n-hexane and the mixed liquor of dichloromethane, and n-hexane and dichloromethane are with 1~2:1
Volume ratio mixing.
4. the detection method of multiple harmful substances, its feature in a kind of fast food wrappers bag according to claim 1
It is：Leaching in the step 2 is supersonic leaching, and the supersonic frequency of ultrasonic generator is 20~40kHz during supersonic leaching,
Ultrasonic power is 120~300W, and the temperature of supersonic leaching is 30~40 DEG C, and the supersonic leaching time is 15~30min, leaching cycle
Number of times is 2~3 times.
5. the detection method of multiple harmful substances, its feature in a kind of fast food wrappers bag according to claim 1
It is：The detailed process of the step 3 is as follows：
The leaching liquid that step 2 is extracted is transferred in rotary evaporation bottle, and Rotary Evaporators are used under 30 DEG C~40 DEG C water bath conditions
Concentration, the leaching liquid volume after concentration is 1/10th of leaching liquid volume before concentration, and the leaching liquid after concentration is shaken into uniform
By 0.22 μm of organic membrane filtration.
6. the detection method of multiple harmful substances, its feature in a kind of fast food wrappers bag according to claim 1
It is：The initial temperature of temperature-rise period in the step 4 in gas chromatography-mass spectrometry work is 30~50 DEG C, keeps 2
~5min, is then warming up to 170~190 DEG C, then be warming up to 250 with 3~5 DEG C/min speed with 5~10 DEG C/min speed
~270 DEG C, 20~25min is kept, finally using Splitless injecting samples, sample size is 1 μ L, and the solvent delay time is 8~15min.
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| CN109738534A (en) * | 2019-01-10 | 2019-05-10 | 安徽省阜阳市国泰彩印包装有限公司 | A kind of color printing packing solvent method for detecting residue |
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