CN106770805A - The assay method of hexene migration amount in a kind of food contact plastic products - Google Patents
The assay method of hexene migration amount in a kind of food contact plastic products Download PDFInfo
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- CN106770805A CN106770805A CN201710121294.7A CN201710121294A CN106770805A CN 106770805 A CN106770805 A CN 106770805A CN 201710121294 A CN201710121294 A CN 201710121294A CN 106770805 A CN106770805 A CN 106770805A
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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
Abstract
The present invention relates to the assay method of hexene migration amount in a kind of food contact plastic products, comprise the following steps：Step S1, sample preparation：Choose polybag sample and the polybag sample of some 10cm × 10cm is fabricated to plastic sealing machine, cleaned with distilled water, dry；It is prepared by step S2, standard working solution and blank test：At least three kinds standard working solutions of concentration that the standard working solution is equipped by hexene；The blank test is the food simulants contacted with negative plastic food packaging materials；It is prepared by step S3, food simulants test solution；Step S4, analysis detection：The standard working solution, blank test and food simulants test solution are determined into hexene migration amount therein using GC-MS.
Description
Technical field
The invention belongs to hexene migration amount in chemical composition detection field, more particularly to a kind of food contact plastic products
Assay method.
Background technology
In modern food production circulation sale system, food contact material has played extremely important effect, can claim
Be " coat " of food, the daily life with us is closely bound up.Especially food contact material plastic products, because of its matter
Gently, it is attractive in appearance, with low cost, insulation, it is resistance to fall, it is corrosion-resistant the advantages of liked by consumers in general.As fruit juice mixer, coffee machine,
Plastic bowl, disposable tableware etc. can be seen everywhere in life, be brought great convenience to us.But people are focusing on life product
But the security of the material that is in contact with food is often ignored while matter.In routine use, harmful substance may from
Migrated to food in the material that food is in contact, and then influence health.The problem has caused extensive concern, every country
The laws and regulations of the food grade materials of correlation, the common the law of food safety for having China, (EC) NO1935/2004 of European Union are put into effect
Food contact material framework regulation, (EU) NO10/2011 European Union intend plastic products regulation, the LFGB foods of Germany contacted with food
Product, commodity and feed code, U.S. FDA 21CFR170-189 parts, No. 370 bulletins of the Health and human services department of Japan etc..Wherein again
It is the most perfect with the food contact material Legal System of European Union.
Hexene has stimulation and anesthetic effect, and headache, cough, expiratory dyspnea are caused after suction；There is maincenter god in a large amount of suctions
Through system suppression, amentia, unconsciousness.Used as one of PP, raw material of PE materials is synthesized, its toxicity is widely known by the people hexene,
People are also increasingly paid close attention to its residual, and use of the European Union to hexene in food contacts plastics and plastic products production is made
Relevant regulations, according to this regulation, the migration amount of food contact plastics analogies must not be higher than 3mg/kg.At present, for food
The detection of hexene migration amount, does not have the method for testing of clear stipulaties in product contact plastic products.
The content of the invention
It is right to solve it is an object of the invention to provide the assay method of hexene migration amount in a kind of food contact plastic products
The technical problem of the detection of hexene migration amount in food contact plastic products.
In order to solve the above-mentioned technical problem, the invention provides the survey of hexene migration amount in a kind of food contact plastic products
Determine method, comprise the following steps：Step S1, sample preparation：Choose polybag sample and be fabricated to plastic sealing machine some
The polybag sample of 10cm × 10cm, is cleaned with distilled water, is dried；It is prepared by step S2, standard working solution and blank test：Institute
State at least three kinds standard working solutions of concentration that standard working solution is equipped by hexene；The blank test is and feminine gender
The food simulants of plastic food packaging materials contact；It is prepared by step S3, food simulants test solution：In different beakers respectively
Load the different food simulants of 200mL, and be preheated to preset temperature；The polybag sample after some drying is taken to fill respectively
Enter in the beaker for filling different food simulants, cover beaker mouthful with preservative film, then beaker is positioned over setting constant temperature
To dry the predetermined time in the baking oven of the preset temperature；Beaker is taken out, adding the food simulants of a certain amount of preheating makes
Food simulants volume is recovered to 200mL in beaker, treats that food simulants are cooled to room temperature, takes in the ml headspace bottle of 5mL to 20mL, incites somebody to action
After lid sealing, food simulants test solution is formed；Step S4, analysis detection：By the standard working solution, blank test and food
Product analogies test solution determines hexene migration amount therein using GC-MS.
Further, the different food simulants include distilled water, olive oil and methanol solution；The i.e. corresponding food
Product analogies test solution includes the examination of aqueous-based food analogies test solution, olive oil food simulants test solution and methanol solution food simulants
Liquid.
Further, the preset temperature is set to 70 DEG C；The predetermined time is set to 2h.
Further, the GC-MS surveys timing condition is as follows：The chromatographic condition for using for：Chromatographic column：DB-5MSDB-624 stones
English capillary column, specification 30m × 0.25mm × 0.25 μm；Injector temperature：150℃；Flow rate of carrier gas is 1.0mL/min；Sample introduction
Amount：1μL；Split sampling, split ratio is 5：1；Temperature programming：The heating gradient be 60 DEG C of initial temperature, keep 5min, after with 5 DEG C/
Min is warming up to 80 DEG C, keeps 3min；Again 230 DEG C are warming up to 30 DEG C/min.
The assay method beneficial effect of hexene migration amount is in food contact plastic products of the invention, measure of the invention
Result is accurate and good stability, and average recovery rate is 82~120%.And assay method is simple to operate, stability is strong, average ten times
Testing standard deviation is not more than 0.065mg/L, with low cost.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is the chromatogram and TIC and mass spectrogram that hexene standard is 1 mcg/ml.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.These accompanying drawings are simplified schematic diagram, only with
Illustration illustrates basic structure of the invention, therefore it only shows the composition relevant with the present invention.
Embodiment 1
The assay method of hexene migration amount, comprises the following steps in a kind of food contact plastic products of the invention：
Step S1, sample preparation：Choose polybag sample and the modeling of some 10cm × 10cm is fabricated to plastic sealing machine
Pocket sample, is cleaned with distilled water, is dried；It is prepared by step S2, standard working solution and blank test：The standard working solution
At least three kinds standard working solutions of concentration being equipped by hexene；The blank test is and negative plastic food packing material
Expect the food simulants of contact；It is prepared by step S3, food simulants test solution：200mL is respectively charged into different beakers different
Food simulants (contacting the ratio of 2mL food simulants according to the contact area of every 1cm × 1cm), and be preheated to default
Temperature；Take the polybag sample after some drying to be respectively charged into the beaker for filling different food simulants, use
Preservative film covers beaker mouthful, then beaker is positioned over sets constant temperature to dry the predetermined time in the baking oven of the preset temperature；Take
Go out beaker, adding the food simulants of a certain amount of preheating makes food simulants volume in beaker recover to 200mL, treats food
Analogies are cooled to room temperature, take in the ml headspace bottle of 5mL to 20mL, after lid is sealed, form food simulants test solution；Step S4,
Analysis detection：The standard working solution, blank test and food simulants test solution are determined into hexene therein using GC-MS
Migration amount.It is as shown in Figure 1 the chromatogram and TIC and mass spectrogram of the mcg/ml of hexene standard 1.
Specifically, the food contact plastic products are used and include PP materials and PE materials.The different food simulation
Thing includes distilled water, olive oil and methanol solution；The i.e. corresponding food simulants test solution is tried including aqueous-based food analogies
Liquid, olive oil food simulants test solution and methanol solution food simulants test solution.
The preparation method of each standard working solution is specially：A () prepares hexene Standard Stock solutions：Accurately weigh content big
In 99.0% hexene standard items 50mg to 100mg volumetric flasks, 0.1mg is accurate to, is dissolved and determined with the methyl alcohol of chromatographically pure rank
Hold, the storing solution seals lucifuge storage at 4 DEG C；B) hexene standard solution is prepared：Pipette 0.100mL hexene standard inventories molten
Liquid is transferred in 100mL volumetric flasks, and with the methanol dilution of chromatographically pure rank to the degree, the content of hexene is 500 μ g/ in solution
L；C () draws appropriate hexene standard solution, matched somebody with somebody with water, 50% methanol solution, 10% methanol solution, olive oil respectively
The standard working solution of 0.3mg/L, 1mg/L, 3mg/L is respectively into concentration.
Optionally, the preset temperature is set to 70 DEG C；The predetermined time is set to 2h.Preset temperature and the time subscribed
Can in the light of actual conditions be adjusted.
It is as follows that the GC-MS surveys timing condition：The chromatographic condition for using for：Chromatographic column：DB-5MS DB-624 quartz capillarys
Tubing string, specification 30m × 0.25mm × 0.25 μm；Injector temperature：150℃；Flow rate of carrier gas is 1.0mL/min；Sample size：1μL；
Split sampling, split ratio is 5：1；Temperature programming：The heating gradient be 60 DEG C of initial temperature, keep 5min, after with 5 DEG C/min heat up
To 80 DEG C, 3min is kept；Again 230 DEG C are warming up to 30 DEG C/min.
The precision and the rate of recovery of this method are detected using additive process.
Choose negative polybag and the negative polybag sample of some 10cm × 10cm is fabricated to plastic sealing machine, with steaming
Distilled water is cleaned, and is dried；Take 10 negative polybag samples to be respectively put into the beaker of 300ml, the water mould of each addition 200mL
Plan thing, then add the working solution of 0.667ml 0.3mg/L, liquid level is marked, covered with preservative film, beaker is positioned over 70
DEG C, baking oven places 2h；Take out at beaker, plus distilled water to reference mark, stirred with glass bar, take the top of 5mL to 20mL
In empty bottle, after lid sealing, hexene migration amount therein is determined using GC-MS, and hexene is in aqueous-based food analogies test solution
Middle TIANZHU XINGNAO Capsul the results are shown in Table 1.
The hexene migration amount (water base analogies) that table 1 is measured using the method for the present invention
| Sample number | Test result (mg/L) | The rate of recovery |
| 1 | 1.00 | 100% |
| 2 | 1.03 | 103% |
| 3 | 1.00 | 100% |
| 4 | 1.08 | 108% |
| 5 | 0.86 | 86% |
| 6 | 0.95 | 95% |
| 7 | 0.97 | 97% |
| 8 | 1.05 | 105% |
| 9 | 1.05 | 105% |
| 10 | 1.05 | 105% |
| Average value | 1.004 | 100.4% |
| Standard deviation | 0.065 | / |
Take the negative polybag sample that 8 PP materials plastic products are made, and be respectively labeled as polybag sample I,
Polybag sample II, polybag sample III, polybag sample IV, polybag sample V, polybag sample VI, polybag sample
VIIth, polybag sample VIII, is respectively and correspondingly placed into and fills the beaker I of 200mL distilled water analogies, fills 200mL distillation Fluid Dynamics
The beaker II of thing, the beaker III for filling the methanol solution analogies that 200mL concentration is 10%, to fill 200mL concentration be 10%
The beaker IV of methanol solution analogies, the beaker V for filling the methanol solution analogies that 200mL concentration is 50%, fill 200mL
Concentration is the beaker VI of 50% methanol solution analogies, fills the beaker VII of 200mL olive oil analogies, fills 200mL olives
In the beaker VIII of olive oil analogies；The standard work that 1mg/L is separately added into beaker I, beaker III, beaker V and beaker VII is molten
Liquid；The standard working solution of 3mg/L is separately added into beaker II, beaker IV, beaker VI and beaker VIII；Mark liquid level,
Covered with preservative film, beaker is positioned over 70 DEG C, baking oven places 2h；Take out at beaker, plus food simulants to reference mark, use
Glass bar stirs, and takes in the ml headspace bottle of 5mL to 20mL, after lid sealing, determines hexene therein using GC-MS and migrates
Amount, and hexene TIANZHU XINGNAO Capsul in each food simulants test solution the results are shown in Table 2.
Hexene migration amount in the plastic products of the PP materials that table 2 is measured using the method for the present invention
Take the polybag sample that 8 PE materials feminine gender plastic products are made, and be respectively labeled as polybag sample I,
Polybag sample II, polybag sample III, polybag sample IV, polybag sample V, polybag sample VI, polybag sample
VIIth, polybag sample VIII, is respectively and correspondingly placed into and fills the beaker I of 200mL distilled water analogies, fills 200mL distillation Fluid Dynamics
The beaker II of thing, the beaker III for filling the methanol solution analogies that 200mL concentration is 10%, to fill 200mL concentration be 10%
The beaker IV of methanol solution analogies, the beaker V for filling the methanol solution analogies that 200mL concentration is 50%, fill 200mL
Concentration is the beaker VI of 50% methanol solution analogies, fills the beaker VII of 200mL olive oil analogies, fills 200mL olives
In the beaker VIII of olive oil analogies；The standard work that 1mg/L is separately added into beaker I, beaker III, beaker V and beaker VII is molten
Liquid；The standard working solution of 3mg/L is separately added into beaker II, beaker IV, beaker VI and beaker VIII；Mark liquid level,
Covered with preservative film, beaker is positioned over 70 DEG C, baking oven places 2h；Take out at beaker, plus food simulants to reference mark, use
Glass bar stirs, and takes in the ml headspace bottle of 5mL to 20mL, after lid sealing, determines hexene therein using GC-MS and migrates
Amount, and hexene TIANZHU XINGNAO Capsul in each food simulants test solution the results are shown in Table 2.
Hexene migration amount in the plastic products of the PE materials that table 3 is measured using the method for the present invention
The analysis result of summary table 1, table 2 and table 3 knows that the average recovery rate of the method for the present invention is 82~120%.
With above-mentioned according to desirable embodiment of the invention as enlightenment, by above-mentioned description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determined according to right.
Claims (4)
1. a kind of food contacts the assay method of hexene migration amount in plastic products, it is characterised in that comprise the following steps：
Step S1, sample preparation：Choose polybag sample and the polybag of some 10cm × 10cm is fabricated to plastic sealing machine
Sample, is cleaned with distilled water, is dried；
It is prepared by step S2, standard working solution and blank test：The standard working solution be equipped by hexene at least three
Plant the standard working solution of concentration；The blank test is the food simulants contacted with negative plastic food packaging materials；
It is prepared by step S3, food simulants test solution：The different food simulants of 200mL are respectively charged into different beakers, and
It is preheated to preset temperature；Take the polybag sample after some drying and be respectively charged into and described fill different food simulants
In beaker, beaker mouthful is covered with preservative film, then beaker is positioned over set constant temperature and make a reservation for dry in the baking oven of the preset temperature
Time；Take out beaker, add a certain amount of preheating food simulants make food simulants volume in beaker recover to
200mL, treats that food simulants are cooled to room temperature, takes in the ml headspace bottle of 5mL to 20mL, after lid is sealed, forms food simulants
Test solution；
Step S4, analysis detection：The standard working solution, blank test and food simulants test solution are determined using GC-MS
Hexene migration amount therein.
2. food as claimed in claim 1 contacts the assay method of hexene migration amount in plastic products, it is characterised in that described
Different food simulants include distilled water, olive oil and methanol solution；I.e.
The corresponding food simulants test solution includes aqueous-based food analogies test solution, olive oil food simulants test solution and methyl alcohol
Solution food simulants test solution.
3. food as claimed in claim 2 contacts the assay method of hexene migration amount in plastic products, it is characterised in that described
Preset temperature is set to 70 DEG C；The predetermined time is set to 2h.
4. food as claimed in claim 3 contacts the assay method of hexene migration amount in plastic products, it is characterised in that described
It is as follows that GC-MS surveys timing condition：
The chromatographic condition for using for：Chromatographic column：DB-5MS DB-624 quartz capillary columns, specification 30m × 0.25mm × 0.25 μ
m；Injector temperature：150℃；Flow rate of carrier gas is 1.0mL/min；Sample size：1μL；Split sampling, split ratio is 5：1；Program liter
Temperature：The heating gradient is 60 DEG C of initial temperature, keeps 5min, after be warming up to 80 DEG C with 5 DEG C/min, keep 3min；Again with 30 DEG C/
Min is warming up to 230 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108680674A (en) * | 2018-05-21 | 2018-10-19 | 深圳天祥质量技术服务有限公司 | 5- ethylidene -2- norbornene specific transfer quantity measuring methods in food contact material |
| CN108760914A (en) * | 2018-05-21 | 2018-11-06 | 深圳天祥质量技术服务有限公司 | TMCD specific transfers quantity measuring method in food contact material |
| CN110031457A (en) * | 2019-04-15 | 2019-07-19 | 深圳安吉尔饮水产业集团有限公司 | The measuring method of ethyl alcohol the amount of migration in a kind of food contact material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108680674A (en) * | 2018-05-21 | 2018-10-19 | 深圳天祥质量技术服务有限公司 | 5- ethylidene -2- norbornene specific transfer quantity measuring methods in food contact material |
| CN108760914A (en) * | 2018-05-21 | 2018-11-06 | 深圳天祥质量技术服务有限公司 | TMCD specific transfers quantity measuring method in food contact material |
| CN110031457A (en) * | 2019-04-15 | 2019-07-19 | 深圳安吉尔饮水产业集团有限公司 | The measuring method of ethyl alcohol the amount of migration in a kind of food contact material |
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