CN102944619A - Method for judging difference of influence of standing and vibrating on phthalic ester transfer volume of paper cup - Google Patents
Method for judging difference of influence of standing and vibrating on phthalic ester transfer volume of paper cup Download PDFInfo
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Abstract
The invention relates to a method for judging difference of influence of standing and vibrating on phthalic ester transfer volume of a paper cup, which belongs to the technical field of analysis and detection. The method comprises the steps of: determining the test index as the transfer volume of phthalic ester in a mouth touch part material of the paper cup; the test factor is the vibrating frequency, which is respectively 0r/min and 80r/min; selecting check test design to design a transfer test scheme; preparing a test sample according to the test scheme; detecting the transfer volume of phthalic ester in the mouth touch part material of the paper cup by pulse unsplit stream sampling and a GC-MS (Gas Chromatography-Mass Spectrometer); detecting detection data by non-parameter tests of two independent samples, wherein the detection method comprises Man-Whitey U detection, and Moses Extreme Reactions; and judging whether remarkable difference of influence of standing and vibrating on phthalic ester transfer volume in the mouth touch part material of the paper cup exists or not. The method has the advantages of ensuring judging and deducing reliability and scientificalness and providing a scientific and accessible systemic method for judging difference of influence of standing and vibrating on phthalic ester transfer volume in the mouth touch part material of the paper cup.
Description
Technical field:
The present invention relates to a kind of standing method of difference that dixie cup phthalate ester migration amount affected with vibration of differentiating, belong to technical field of analysis and detection.
Background technology:
Phthalate ester, also be phthalic ester (PAEs), refers to the esterification derivative of phthalic acid (Phthalate acid), is plasticiser the most common in plastic cement industry.In the daily and industrial production that is widely used in the high molecular weight plastic product, as Polyvinylchloride (PVC), polypropylene (PP), foam, also can make an addition in adhesive, coating, printing ink.
Phthalic ester (PAEs) is included into the endocrine of key monitoring in the world and disturbs hormone or Environmental Hormone in recent years.European Union, the U.S. etc. classify PAEs as priority pollutants, and constantly increase the monitoring kind.In " Chinese environmental priority pollutant blacklist " also listed DMP, DBP and tri-kinds of phthalic esters of DOP by China
[1].Ministry of Health of the People's Republic of China, in issue on June 1st, 2011 emergency notice " bulletin of the food additives list (the 6th batch) of the non-edible material from soybeans of the illegal interpolation of possibility and easy abuse in about announcement food " (Ministry of Public Health announces 2011 No. 16), classifies 17 kinds of phthalic esters as the 6th batch of illegal food additives.The PAEs kind of international, domestic key monitoring is in Table 1.
The PAEs kind of table 1 world, domestic key monitoring
The regulation of contained adjuvant Special migration in the food contact material has been introduced in European Union's 2002/72/EC instruction
[2].The 2007/19/EC instruction was stipulated from 1 day June in 2008, if the plastifier in Food Contact plastic material and goods does not meet the limit index in table 2, European Union will forbid producing and this product of import.In GB 9685-2008 that China newly issues according to " Food Hygiene Law of the People's Republic of China " " food containers, wrappage used additives are used hygienic standard ", the relevant regulations of relevant plastifier is as table 3
[2].
The limit index relevant to plastifier in the 2007/19/EC of table 2 European Union instruction
The regulation relevant to plastifier in table 3 GB 9685-2008
Dixie cup is that the body paper that will make with wood pulp carries out machining, bonding a kind of paper container of doing, and outward appearance is cup shape.Dixie cup, aborning in order to reach the water proof effect, can be coated with the layer of polyethylene water-separating film at inwall
[3,4].Tygon is one of safest chemical substance in food processing.Phthalate ester only is applied to Polyvinylchloride in theory, should not exist in tygon.But the recovery again of plastics is used, and adds unclear classification, causes in some vinyon and contains a small amount of phthalate ester
[5], secondly, if the dixie cup water-separating film is used industrial plastic, in order to increase cup toughness and rigidity, also can add plastifier.If additive capacity is excessive or use illegal plastifier, sanitary condition to be difficult to guarantee
[3].
Moreover, have in riotous profusion pattern and the printed words of ink printing on some dixie cups, when dixie cup stacks, the printing ink of dixie cup outside must affect the dixie cup internal layer that wrap up its outside
[3].Lip contact rim of a cup while drinking water, printed patterns printing ink used may be ingested
[3].Tradition heat-set ink principal ingredient is polyvinyl chloride resin, phthalate plasticizers, pigment and auxiliary agent, and in its product, the content of phthalic ester receives publicity in recent years, and more and more is subject to various strict limiting the quantity of and regulates
[6].
In addition, in the adhesion technique of dixie cup, glue is the most frequently used bonding agent.The people such as Lai Ying
[7]adopt GC-MS to detect dibutyl phthalate (DBP) in certain white glue with vinyl.The people such as Yang Bin
[8]the same GC-MS that adopts detects dibutyl phthalate (DBP) and diisobutyl phthalate (DIBP) in certain water base adhesive.
As can be seen here, dixie cup water-separating film used, printing-ink, bonding agent may be all the main sources that dixie cup is polluted by phthalic ester.
Measure in the world the method for migration volume of chemical substances in packaging material for food normally according to the feature of food, select different simulation solvent (also claiming the food analogies), tested under given conditions, with the stripping quantity of material, mean the migration amount
[9 ~ 11].Accordingly, but simulating oral cavity environment, and the amount of touching phthalate ester in the part material with the paper cup rim of saliva analogies stripping means that paper cup rim touches phthalate ester in the part material and, to the migration amount in oral cavity, is called for short dixie cup phthalate ester migration amount.
The annual Disposable paper cup consumed of China reaches more than 50,000,000,000, and increases progressively situation along with the raising of national consumption level presents.Carry out phthalate ester in the dixie cup contacted with oral cavity and, to the research of oral cavity migration situation, set up effective analytical approach of phthalate ester migration amount in the dixie cup contacted with oral cavity, can be for assessment, supervision paper cup lifting for data and theory support.
For sentencing in the migration test of any packaging material for food, have plenty of under standing condition and carry out
[10 ~ 13], have plenty of under oscillating condition and carry out
[14 ~ 17].Many about the standing impact comparison with vibrating on the migration amount, only by the comparison directly perceived of simple broken line graph analysis or data
[14 ~ 17]draw the simple knot opinion, the fluctuation that the change of test condition can't be brought impact and the test error of migration amount is distinguished, and has affected the accuracy of transition condition the selection result and follow-up migration quantitative determination result.So far, the non-parametric test at home and abroad had no about adopting two independent samples is analyzed test figure, and differentiates the standing open report of the method for difference that dixie cup phthalate ester migration amount affected with vibration according to analysis result.
List of references:
[1] Chen Zhuling, Huang Yukui ，Wang Gui Mei etc. Phthalates of Environment Hormone in Cosmetics detection method research [J]. Environmental science and technology. 2007,30 (4): 43-47.
[2] Shi Wancong. the toxicity of plastifier and relevant limit rules [J]. additives for plastics, 2010,3:43-47.
[3]
http://baike.baidu.com/view/704637.htm
[4]http://baike.baidu.com/view/289346.htm
[5]?http://groups.google.com/group/ntusunrise_file/tree/browse_frm/month/2011-06/df4fe11ed0b55e64?hide_quotes=no
[6] Chen Hongwei, Liao Liang, Luo Qun. the phthalate in gas chromatography determination printing ink [J]. Guangdong chemical industry, 2011, (7), 136 ~ 140.
[7] Lai Ying. GC-MS is measured benzene homologues and phthalic ester plasticizer [J] in adhesive for building simultaneously. assay laboratory, 2010, (3), 58 ~ 62.
[8] Yang Bin, Chen Chaoying, Wu Da, woods Hua Qing, Chen Xingjie, Dai Yunhui. combined gas chromatography mass spectrometry is measured the phthalic ester [J] in the aqua type latex for cigarette. tobacco chemistry, 2011, (7), 48-51.
[9] Wang Shiping. food safety detection technology [M]. China Agricultyre University Press (Beijing), August in 2009 the 1st edition: 280.
[10] guide [S] that in GB/T 23296.1-2009 food contact material plastics, in the restricted substances plastics, material is selected to food and food analogies specific transfer test method and assay and food analogies condition.
[11] guide [S] that in SN/T 2280-2009 food contact material plastics, in the restricted substances plastics, material is selected to food and food analogies specific transfer test method and assay and food analogies condition.
[12] analytical approach [S] of the mensuration gas chromatography-MS of phthalic ester plasticizer migration amount in the plastic molded article of SN/T 2037-2007 People's Republic of China (PRC) inspection and quarantining for import/export industry standard and Food Contact.
[13] Sun Chunyun, Zhang Kerong, Cheng little Yan, Zheng Bo. the stripping experiment [J] to 7 kinds of environmental estrogens in plastic toy of simulated sweat and saliva. Chinese Journal of Health Laboratory Technology, 2006,16(1): 32-34.
[14] bang literary composition, Lin Shaojie, Liu Qu, Liu Li. seven kinds of environmental estrogens of plastic toy are at simulated sweat and saliva stripping behavioral study [J], Tropical China medical science, 2006,6(1), 39 ~ 41.
[15] Yu Ye, Wang Xin, Sun Li, Dong Hua. in plastic products, phthalate ester is to the research [J] of food analogies migration. food science and technology, 2008,33(12), 117 ~ 119.
[16] Yang Zuojun, Wang Chengyun, Zhang Weiya, Lan Fang, Xie Liqi. the migratory behaviour research [J] of phthalic ester plasticizer in body fluid in the PVC plastics. Polyvinylchloride, 2006, (2), 23 ~ 30.
[17] Niu Zengyuan, Fang Liping ，Yang osmanthus friend, Xue Qiuhong, Wang Jingtang, Sun Zhongsong. the migration [J] of Phthalates of Environment Hormone in the synthetic perspiration in textile. textile journal, 2006,27(2), 74 ~ 77.
[18] Yang De. test design and analysis [M]. Beijing: Chinese agriculture publishing house, 2002,64 ~ 79.
[19] Su Jinming. statistic software SPSS 12.0 for Windows application and development guides ［ M ］. Beijing: Electronic Industry Press, 2004,253 ~ 259.
[20] Lu Wendai. SPSS statistical study (the 4th edition) ［ M ］. Beijing: Electronic Industry Press, 2010.
[21] GB/T 16886.15-2003/ISO 10993-15:2000 medicine equipment biological evaluation [S].
[22] mensuration of GB/T 21911-2008 Phthalic Acid Esters in Food [S].
Summary of the invention:
The object of the present invention is to provide a kind of standing method of difference that dixie cup phthalate ester migration amount affected with vibration of differentiating.
The present invention means that with the amount of phthalate ester in the tactile part material of the paper cup rim of saliva analogies stripping paper cup rim touches phthalate ester in the part material and, to the migration amount in oral cavity, is called for short dixie cup phthalate ester migration amount.The design of employing control test
[18]carry out respectively migration test under standing or oscillating condition, by the non-parametric test of two independent samples
[19,20], set up " differentiating the standing method of difference that dixie cup phthalate ester migration amount affected with vibration ", thereby guaranteed reliability and the science differentiating, infer.
In statistics, the significance test of difference of two independent samples is only to meet sample separate, and just can carry out the t check during Normal Distribution condition.Therefore, before t check, at first need the sample to carrying out the average comparison to make independence test and normal distribution-test, and then according to variance neat with uneven two kinds of situations, apply different t statistics and test.Otherwise, carry out by force the t check conclusion that easily makes the mistake.
Can not meet in data under the condition of this parametric test, need to select the non-parametric test method
[19,20].With parametric technique, compare, nonparametric technique have distribute freely, can be used for by the numerical value meaning say strict but have certain hierarchal order data analysis and calculate simple three large advantages.The non-parametric test of two independent samples, comprise Mann-Whitney U check (rank test, both be suitable for small sample, also be applicable to large sample), Moses Extreme Reactions(extremely reacts check, be applicable to small sample), Kolmogorov-Smirnov Z(K-S check, be applicable to large sample), Wald-Wolfowitz runs(runs test, be applicable to large sample).Whether according to the non-parametric test result of two independent samples, can differentiate two samples has significant difference or no from same overall
[19,20].
The standing method of difference that dixie cup phthalate ester migration amount affected with vibration of differentiation provided by the invention, concrete steps are as follows:
(1) confirmed test index is the migration amount that paper cup rim touches phthalate ester in the part material, and unit is μ g/3 pcs;
(2) the confirmed test factor and level thereof: test factor is oscillation frequency, and its level is respectively 0 r/min and 80 r/min two levels;
(3) select the control test design to carry out the migration test conceptual design;
(4) according to testing program, preparation detects and uses sample;
(5) adopt pulse Splitless injecting samples, GC-MS test paper rim of a cup to touch the migration amount of phthalate ester in the part material;
(6) adopt the non-parametric test of two independent samples to test to detecting data, the method for inspection is Mann-Whitey U check, and Moses Extreme Reactions check;
(7) whether there were significant differences to differentiate the standing impact with vibrating on phthalate ester migration amount in the tactile part material of paper cup rim according to assay.
The invention has the advantages that:
A. whether there were significant differences to differentiate the standing impact with vibrating on phthalate ester migration amount in the tactile part material of paper cup rim according to the non-parametric test result of two independent samples, can guarantee reliability and the science differentiating, infer;
B. paper cup rim is touched the impact of phthalate ester migration amount in the part material whether there were significant differences provide a kind of science feasible systems approach for differentiating standing and vibration;
Embodiment:
Below in conjunction with example, the present invention is described in detail, but do not limit the present invention.
The present invention adopts Mann-Whitney U check (rank test) and Moses Extreme Reactions(extremely to react check) differentiate standing difference dixie cup phthalate ester migration amount affected with vibration, concrete steps are as follows:
1 confirmed test index
Test index is the migration amount that paper cup rim touches phthalate ester in the part material, and unit is μ g/3 pcs.
The 2 confirmed test factor and levels thereof
Test factor is oscillation frequency, and its level is respectively 0 r/min and 80 r/min two levels.
3 select the control test design to carry out migration test conceptual design (table 4)
The control test scheme of table 4 migration test
A, saliva analogies formulas (pH 7.58): every liter of ultrapure water (three grades of water) phosphoric acid disodium hydrogen (Na2HPO4) 0.260 g, sodium chloride (NaCl) 0.700 g, potassium rhodanide (KSCN) 0.330 g, potassium dihydrogen phosphate (KH2PO4) 0.200 g, sodium bicarbonate (NaHCO3) 1.500 g, potassium chloride (KCl) 1.200 g[21].
4 according to testing program preparation detection sample
According to testing program (table 4), randomly draw 18 of the dixie cups of same brand and specification, under cutting out at 15 mm places, distance rim of a cup edge respectively, corresponding mouthful of tactile part material, as test material, amounts to 18.Every 9 is 1 group, and totally 2 groups, 1 group is used for standing migration test, and another 1 group is used for vibrating migration test.Calculate the area of every test material, and as mouth tactile area (0.33 dm of each dixie cup
2/ pcs).
1 analogizes 9] cause.Different saliva analogies touch the impact of part phthalate ester migration amount phthalic ester mixed standard solution (each composition of phthalic ester is in Table 1) 1 mL that each constituent concentration is 20 mg/L that gets on paper cup rim, in 250 mL conical flasks, volatilizees fully with nitrogen blowing to solvent normal hexane.Inject area-volume ratio 1 dm that saliva analogies 150 mL(press the tactile part material of paper cup rim and saliva analogies again in each conical flask
2/ 50 mL, convert with it and obtain the saliva analogies volume that test should add with the area of 9 test materials).
In the vibration migration test, the above-mentioned conical flask that phthalic ester mixed standard solution and 150 mL saliva analogies are housed is placed in to isothermal vibration device balance to 37 ℃ ± 1 ℃.By 9 test materials that cut be placed in the saliva analogies that constant temperature is good (temperature: 37 ℃ ± 1 ℃, oscillation frequency: 80 r/min), 30 min that vibrate ± 1 min.Afterwards, saliva analogies extract being transferred to while hot to sealing in conical flask preserves.After liquid to be extracted is got back to room temperature, accurately measure and be equivalent to tactile extract 50 mL partly of 3 paper cup rims in 125 mL separating funnels, and add benzoic acid Bian ester (interior mark) solution 1 mL of 0.5 mg/L, with 3 times (each 30 mL) of chromatographic pure dichloromethane extraction.Merge organic phase, add a small amount of anhydrous sodium sulfate drying to spend the night.Be concentrated near doing with Rotary Evaporators, then it is to be detected to be settled to 1 mL with normal hexane.
The migration test of vibrating in the same way repeats 6 times altogether, and 1 blank sample is made in each test simultaneously, and the difference of blank sample and test specimen is not add the phthalic ester mixed standard solution in the blank sample system.
The sample preparation methods of standing migration test is substantially identical with the sample preparation methods of vibration migration test, and difference is that the oscillation frequency of isothermal vibration device in standing migration test is made as 0 r/min from start to finish.
In the same way standing migration test is repeated 6 times altogether, 1 blank sample is made in each test simultaneously, and the difference of blank sample and test specimen is not add the phthalic ester mixed standard solution in the blank sample system.
5 adopt pulse Splitless injecting samples, GC-MS test paper rim of a cup to touch the migration amount of phthalate ester in the part material
All samples pulse Splitless injecting samples, GC-MS detects
[22]the amount of phthalate ester in made sample, and mean phthalate ester migration amount in each tactile part material of test institute's paper cup rim of being surveyed with this, testing result is in Table 5.Because every kind of test repeats 6 times altogether by scheme, obtain 6 samples, each sample is duplicate detection 2 times again, and therefore different migration tests can obtain 12 different data for different phthalate esters, and 12 data are done one group, and every group of data are exactly a sample.As, detecting and obtain 12 different data for DMP in standing migration test, these 12 data are sample 1; Also detect and obtain 12 different data for DMP in the vibration migration test, these 12 data are sample 2; By that analogy.
Table 5 paper cup rim touches phthalate ester migration amount in the part material and detects data
b(μ g/3 pcs)
B, the contained 18 kinds of phthalate ester concentration of mixed standard solution of using due to this test equate, and the detectability of diisononyl phthalate (DINP) and diisooctyl phthalate (DIDP) is than 1 order of magnitude of the detection limit for height of other phthalate material, therefore fails to detect and obtain diisononyl phthalate (DINP) and diisooctyl phthalate (DIDP) related data.
6 Mann-Whitney U checks (rank test)
The Mann-Whitney U check (rank test) of two independent samples can be for the ratio judgement of two population distribution.It is one of the strongest non-parametric test, is applicable to small sample and large sample test simultaneously.Its null hypothesis: two independent samples from two population distribution without two samples of significance difference XOR from same overall.
Mann-Whitney U check (rank test) realizes judgement by the research to two groups of sample mean orders.Order simply says to be exactly the ranking of variate-value sequence, data can be arranged by ascending order, and each variate-value can have position or a ranking in whole variate-value sequence, and this position or ranking are exactly the order of variate-value.
Adopt the Mann-Whitney U of existing two independent samples to check standing in (rank test) analytical table 5 and vibration migration amount detection data.According to assay, can infer for different phthalic esters, whether standing migration and two samples of vibration migration have significant difference or no from same overall, the results are shown in Table 6 ~ 7.
Table 6 Mann-Whitney U check order table
Table 7 Mann-Whitney U assay
d
C, do not proofread and correct;
D, the grouping variable: standing, vibration
;
In table 7, DMP, DIBP, DBP, DMEP, DEEP, DPP, DHXP, BBP, DBEP, DCHP, DPHP, DNOP, the approximate significance probability Asymp. Sig.(2-tailed of DNP) and accurate significance probability Exact Sig. [2*(1-tailed Sig.)] all be less than 0.05, can judge: standing and two kinds of transition conditions of vibration touch DMP in the part material to paper cup rim, DIBP, DBP, DMEP, DEEP, DPP, DHXP, BBP, DBEP, DCHP, DPHP, DNOP, there were significant differences in the impact of DNP migration amount.In addition, the approximate significance probability Asymp. Sig. (2-tailed) of DEP, BMPP, DEHP migration amount and PAEs gross migration and accurate significance probability Exact Sig. [2*(1-tailed Sig.)] all be greater than 0.05, can judge: standing and two kinds of transition conditions of vibration touch DEP in the part material to paper cup rim, BMPP, the impact of DEHP migration amount and PAEs gross migration does not have significant difference.
7 Moses Extreme Reactions(extremely react check)
Moses Extreme Reactions(extremely reacts check) from two independent samples of another angle check from two population distribution whether have significant difference.Its null hypothesis: two independent samples from two population distribution without significant difference.Basic thought: by one group of sample sample in contrast, another group sample is as test sample, and whether the check test sample extreme reaction occurred with respect to check sample.If extreme reaction does not appear in test sample, think that two population distribution, without significant difference, think and have significant difference on the contrary.
Adopt the Moses Extreme Reactions(of existing two independent samples extremely to react check) standingly in analytical table 5 with vibration migration amount, detect data.Whether have significant difference or no from same overall, the results are shown in Table 8 ~ 9 if according to analysis result, can differentiate two samples.
Table 8 Moses Extreme Reactions checks frequency table
Table 9 Moses Extreme Reactions assay
e
E, the grouping variable: vibration, standing;
Due in table 9, utilize DIBP, DBP, the significance probability Sig.(1-tailed that whole sample datas of DBEP calculate) and the significance probability Sig.(1-tailed calculated through sample data after rejecting) all be less than 0.05, can judge: there were significant differences on the impact of DIBP, DBP, DBEP migration amount in the tactile part material of paper cup rim for standing and two kinds of transition conditions of vibration.In addition, utilize DMP, DEP, DMEP, BMPP, DEEP, DPP, DHXP, BBP, DCHP, DEHP, DPHP, DNOP, the significance probability Sig.(1-tailed that whole sample datas of DNP migration amount and PAEs gross migration calculate) and the significance probability Sig.(1-tailed calculated through sample data after rejecting) all be greater than 0.05, can judge: standing and two kinds of transition conditions of vibration touch DMP in the part material to paper cup rim, DEP, DMEP, BMPP, DEEP, DPP, DHXP, BBP, DCHP, DEHP, DPHP, DNOP, the impact of DNP migration amount and PAEs gross migration does not have significant difference.
8 differentiate the standing impact with vibrating on phthalate ester migration amount in the tactile part material of paper cup rim according to assay, and whether there were significant differences.
Comprehensive Mann-Whitney U check (rank test) and Moses Extreme Reactions(extremely react check) result can judge: standing with vibrate that there were significant differences in the impact of two kinds of transition conditions on DIBP, DBP, DBEP migration amount in the tactile part material of paper cup rim, and the data by DIBP, DBP, tri-kinds of phthalate ester migration amounts of DBEP in table 5 can be found out, migration amount when in the tactile part material of the paper cup rim of standing processing, the migration amount of phthalate ester is higher than oscillation treatment.In addition, standingly with two kinds of transition conditions of vibration, paper cup rim is touched to DEP in the part material, BMPP, the impact of the phthalate ester migration amount such as DEHP and PAEs gross migration does not have significant difference.
Claims (1)
1. differentiate the standing method of difference that dixie cup phthalate ester migration amount affected with vibration for one kind, it is characterized in that the concrete steps of the method are as follows:
(1) confirmed test index is the migration amount that paper cup rim touches phthalate ester in the part material, and unit is μ g/3 pcs;
(2) the confirmed test factor and level thereof: test factor is oscillation frequency, and its level is respectively 0 r/min and 80 r/min two levels;
(3) select the control test design to carry out the migration test conceptual design;
(4) according to testing program, preparation detects and uses sample;
(5) adopt pulse Splitless injecting samples, GC-MS test paper rim of a cup to touch the migration amount of phthalate ester in the part material;
(6) adopt the non-parametric test of two independent samples to test to detecting data, the method for inspection is Mann-Whitey U check, and Moses Extreme Reactions check;
(7) whether there were significant differences to differentiate the standing impact with vibrating on phthalate ester migration amount in the tactile part material of paper cup rim according to assay.
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