CN102914614B - Method for screening saliva stimulant influencing transfer volume of phthalate in paper cup mouth touching material - Google Patents
Method for screening saliva stimulant influencing transfer volume of phthalate in paper cup mouth touching material Download PDFInfo
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Abstract
The invention relates to a method for screening a saliva stimulant influencing a transfer volume of phthalate in a paper cup mouth touching material, belonging to the technical field of analysis and detection. The method comprises the contents that: the test index is the transfer volume of the phthalate in the paper cup mouth touching material; the test factors are five different saliva stimulants; the test result processing is to perform approximating variance analysis by adopting Welch and Brown-Forsythe ways; and the Tamhane, Dunnett T3 and Games-Howell and Dunnett C inspections are adopted for multiple comparisons so as to judge the degree of the influence from different saliva stimulants to the transfer volume of the phthalate in the paper cup mouth touching material, thereby screening out an optimal saliva stimulant. The method for screening the saliva stimulant influencing the transfer volume of the phthalate in the paper cup mouth touching material, disclosed by the invention, has the advantages of judging whether the influence from different saliva stimulants to the transfer volume of the phthalate in the paper cup mouth touching material is outstanding, deducing the difference of the influence from different saliva stimulants to the transfer volume of the phthalate in the paper cup mouth touching material, directly analyzing an influence trend, judging and deducing scientifically and reliably, and providing data and theoretical support for monitoring the paper cup.
Description
Technical field:
The present invention relates to a kind of screening and affect the method that paper cup rim touches the saliva analogies of material phthalate ester migration amount, belong to technical field of analysis and detection.
Background technology:
Phthalate ester, is also 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 being widely used in high molecular weight plastic product, as Polyvinylchloride (PVC), polypropylene (PP), foam, also can make an addition in adhesive, coating, ink.
Phthalic ester (PAEs) is included into endocrine disruption hormone or the Environmental Hormone of key monitoring in the world in recent years.PAEs is classified as priority pollutants by European Union, the U.S. etc., and constantly increases monitoring kind.DMP, DBP and DOP tri-kinds of phthalic esters are also listed in " Chinese environmental priority pollutant blacklist " by China
[1].Ministry of Health of the People's Republic of China issues emergency notice " bulletin about the food additives list (the 6th batch) of the non-edible material from soybeans and easy abuse of announcing the illegal interpolation of possibility in food " (Ministry of Public Health announces 2011 No. 16) on June 1st, 2011,17 kinds of phthalic esters is classified as the 6th batch of illegal food additives.The PAEs kind of international, domestic key monitoring is in table 1.
Table 1 is international, the PAEs kind of domestic key monitoring
European Union's 2002/72/EC instruction introduces the regulation of contained adjuvant Special migration in food contact material
[2].2007/19/EC directives prescribe was 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 import this product.About the relevant regulations of plastifier is as table 3 in the GB 9685-2008 " food containers, wrappage used additives use hygienic standard " that China newly issues according to " Food Hygiene Law of the People's Republic of China "
[2].
Limit index relevant to plastifier in table 2 European Union 2007/19/EC instruction
Regulation relevant to plastifier in table 3 GB 9685-2008
Dixie cup be the body paper made with wood pulp is carried out machining, bonding a kind of paper container of doing, outward appearance is cup shape.Dixie cup, aborning in order to reach water proof effect, can be coated with layer of polyethylene water-separating film at inwall
[3,4].Tygon is one of safest chemical substance in food processing.Phthalate ester is only applied to Polyvinylchloride in theory, should not exist in tygon.But the recovery again of plastics uses, and adds unclear classification, cause in some vinyon containing a small amount of phthalate ester
[5], secondly, if dixie cup water-separating film uses industrial plastic, in order to increase cup toughness and rigidity, also can plastifier be added.If additive capacity is excessive or use illegal plastifier, sanitary condition is difficult to ensure
[3].
Moreover some dixie cups have in riotous profusion pattern and the printed words of ink printing, when dixie cup stacks, the ink outside dixie cup must affect the dixie cup internal layer wrapped up outside it
[3].Lip contact rim of a cup when drinking water, printed patterns 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 is more and more subject to various limitation strictly 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 in certain white glue with vinyl, detect dibutyl phthalate (DBP).The people such as Yang Bin
[8]same employing GC-MS 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 the method for migration volume of chemical substances in packaging material for food in the world normally according to the feature of food, select different simulation solvents (also claiming food simulants), test under given conditions, represent migration amount with the stripping quantity of material
[9 ~ 11].Accordingly, can simulating oral cavity environment, touch the amount of phthalate ester in portion of material with the paper cup rim of saliva analogies stripping to represent that paper cup rim touches phthalate ester in portion of material and, to the migration amount in oral cavity, is called for short paper cup rim and touches material phthalate ester migration amount.
The Disposable paper cup that China consumes every year 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 with oral contact and, to the research of oral cavity migration situation, set up effective analytical approach of phthalate ester migration amount in the dixie cup with oral contact, can for assessment, supervision paper cup lifting be for data and theory support.
For protecting consumers in general to greatest extent, when analyzing paper cup rim and touching phthalate ester in portion of material to the migration amount in oral cavity, reality to be simulated as far as possible and making migration amount maximum.When carrying out simulation migration test, the selection of saliva analogies kind is the emphasis that those skilled in the art pay close attention to.Scientific and rational saliva analogies are determined in screening, and specification sample preparation technology ensures that follow-up paper cup rim touches the key of phthalate ester migration quantitative determination result reliability and science in portion of material.
So far, at home and abroad have no about screening affect the open report that paper cup rim touches the method for the saliva analogies of phthalate ester migration amount in material.
List of references
[1] Chen Zhuling, Huang Yukui, Wang Guimei 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 statute of limitation [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 [J] in gas chromatography determination ink. Guangdong chemical industry, 2011, (7), 136 ~ 140.
[7] Lai Ying. benzene homologues and phthalic ester plasticizer [J] in GC-MS Simultaneously test adhesive for building. 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 measures the phthalic ester [J] of cigarette in aqua type latex. tobacco chemistry, 2011, (7), 48-51.
[9] Wang Shiping. food safety detection technology [M]. China Agricultyre University Press (Beijing), August the 1st edition: 280. in 2009
[10] guide [S] that in GB/T 23296.1-2009 food contact material plastics, in restricted substances plastics, material is selected to food and food simulants specific transfer test method and assay and food simulants condition.
[11] guide [S] that in SN/T 2280-2009 food contact material plastics, in restricted substances plastics, material is selected to food and food simulants specific transfer test method and assay and food simulants condition.
[12] Lin Weixuan, Huang Chun, Li Zhixi, etc. test design method [M]. Dalian: publishing house of the Maritime Affairs University Of Dalian, 1995,146 ~ 154.
[13] Ren Luquan. testing pressure coefficient and analysis (second edition) [M]. Beijing: Higher Education Publishing House, 2003,107 ~ 108.
[14] cogongrass poem pine, Zhou Jixiang, Chen Ying. test design [M]. Beijing: China Statistics Press, 2004,138 ~ 144.
[15] Yang De. test design and analysis [M]. Beijing: Chinese agriculture publishing house, 2002,64 ~ 79.
[16] mensuration [S] of GB/T 21911-2008 Phthalic Acid Esters in Food.
[17] Su Jinming. statistic software SPSS 12.0 for Windows applies and development guides ［ M ］. Beijing: Electronic Industry Press, 2004,253 ~ 259.
[18] Lu Wendai. SPSS statistical study (the 4th edition) ［ M ］. Beijing: Electronic Industry Press, 2010.
Summary of the invention:
A kind of screening is the object of the present invention is to provide to affect the method that paper cup rim touches the saliva analogies of material phthalate ester migration amount.
The present invention adopts representative saliva analogies, and in conjunction with single-factor random test design, approximating variances analysis, F significance test, Multiple range test, establishing a kind of screening affects the method that paper cup rim touches the saliva analogies of material phthalate ester migration amount.Raising dixie cup Product quality and safety is had important practical significance.
The concrete steps of the inventive method are as follows:
(1) determine that test index is the migration amount that paper cup rim touches phthalate ester in portion of material, unit is μ g/3 pcs;
(2) test factor and level thereof is determined: saliva analogies kind, 5 levels;
(3) single-factor Random Design is selected to work out testing program;
(4) detection sample is prepared according to testing program;
(5) adopt pulse Splitless injecting samples, migration amount that GC-MS test paper rim of a cup touches phthalate ester in portion of material;
(6) homogeneity test of variance is carried out to detection data;
(7) if sample variance is uneven, Welch and Brown-Forsythe two kinds of methods are adopted to carry out approximating variances analysis, F significance test to detection data;
(8) on the test index having appreciable impact, adopt Tamhane, Dunnett T3, Games-Howell and Dunnett C checks 4 kinds of methods to carry out Multiple range test to detection data;
(9) differentiate that different saliva analogies touch the influence degree of phthalate ester migration amount in portion of material to paper cup rim according to analysis result;
(10) touch phthalate ester migration amount average in portion of material according to the paper cup rim of each sample, draw Average value compare figure, and paper cup rim is touched to the effect tendency of phthalate ester migration amount in portion of material according to Average value compare figure intuitive analysis different saliva analogies;
(11) determine to measure the best saliva analogies that paper cup rim touches phthalate ester migration amount in portion of material.
The advantage of the inventive method is:
A. by approximating variances analysis and F significance test, can differentiate that whether the impact that different saliva analogies touch phthalate ester migration amount in portion of material to paper cup rim is remarkable;
B. by Multiple range test can infer between the process of different saliva analogies, phthalate ester migration amount in portion of material touched on paper cup rim affect difference;
C. by Average value compare figure energy intuitive analysis different saliva analogies, paper cup rim is touched to the effect tendency of phthalate ester migration amount in portion of material;
D. for differentiating that different saliva analogies touch the impact of phthalate ester migration amount in portion of material to paper cup rim and screen best saliva analogies, the system approach that a kind of science is feasible is provided.
Accompanying drawing illustrates:
Fig. 1 is the Average value compare figure that different saliva analogies affect repefral (DMP) migration amount.
Fig. 2 is the Average value compare figure that different saliva analogies affect diethyl phthalate (DEP) migration amount.
Fig. 3 is the Average value compare figure that different saliva analogies affect diisobutyl phthalate (DIBP) migration amount.
Fig. 4 is the Average value compare figure that different saliva analogies affect n-butyl phthalate (DBP) migration amount.
Fig. 5 is the Average value compare figure that different saliva analogies affect dimethyl glycol phthalate (DMEP) migration amount.
Fig. 6 is the Average value compare figure that different saliva analogies affect phthalic acid two-4-methyl-2-amyl group ester (BMPP) migration amount.
Fig. 7 is the Average value compare figure that different saliva analogies affect phthalic acid two (2-ethoxyethyl group) ester (DEEP) migration amount.
Fig. 8 is the Average value compare figure that different saliva analogies affect amyl phthalate (DPP) migration amount.
Fig. 9 is the Average value compare figure that different saliva analogies affect dihexylphthalate (DHXP) migration amount.
Figure 10 is the Average value compare figure that different saliva analogies affect butyl benzyl phthalate (BBP) migration amount.
Figure 11 is the Average value compare figure that different saliva analogies affect phthalic acid two (2-butoxyethyl group) ester (DBEP) migration amount.
Figure 12 is the Average value compare figure that different saliva analogies affect phthalic acid two (2-ethylhexyl) ester (DEHP) migration amount.
Figure 13 is the Average value compare figure that different saliva analogies affect diphenyl phthalate (DPHP) migration amount.
Figure 14 is the Average value compare figure that different saliva analogies affect phthalic acid positive ester (DNP) migration in two ninth of the ten Heavenly Stems amount.
Figure 15 is the Average value compare figure that different saliva analogies affect phthalic ester (PAEs) gross migration.
Embodiment:
Below in conjunction with accompanying drawing, the present invention is described in detail, but do not limit the present invention.
Screening affects paper cup rim, and to touch the method step of the saliva analogies of phthalate ester migration amount in material as follows:
1 determines test index
Determine that test index is the migration amount (each composition of phthalate ester is in table 1) that paper cup rim touches phthalate ester in portion of material, unit is μ g/3 pcs.
2 determine test factor and level thereof
Determine that test factor is saliva analogies kinds.Data-searching shows, at nearly 5 kinds with authoritative saliva analogies, so saliva analogies number of levels is 5 levels (see table 4 and annotations thereof).
3 select single-factor Random Design
[12 ~ 15]establishment testing program (table 4)
Table 4 screens the single-factor Random Design testing program of saliva analogies kind
A, test solution 1 (pH 2.50): test solution ultrapure water (tertiary effluent) preparation, often liter of sodium chloride-containing (NaCl) 4.5 g, potassium chloride (KCl) 0.3 g, sodium sulphate (Na
2sO
4) 0.3 g, ammonium chloride (NH
4cl) 0.4 g, lactic acid [CH
3cH(OH) COOH] 3.0 g, urea (H
2nCONH
2) 0.2 g. imports and exports saliva of textile colour fastness experimental technique [S] see SN/T 1058 – 2002.
B, test solution 2 (pH 6.40): ultrapure water (tertiary effluent). see Germany's " food, tobacco product, cosmetics and other commodity administrative law ".
C, test solution 3 (pH 6.80): test solution ultrapure water (tertiary effluent) preparation, often liter containing Magnesium dichloride hexahydrate (MgCl
2 .6H
2o) 0.17 g, CALCIUM CHLORIDE DIHYDRATE (CaCl
2 .2H
2o) 0.15 g, two hypophosphite monohydrate hydrogen dipotassium (K
2hPO
4 .2H
2o) 0.76 g, sal tartari (K
2cO
3) 0.53 g, sodium chloride (NaCl) 0.33 g, potassium chloride (KCl) 0.75 g, regulate pH to 6.80 ± 0.1, see the mensuration [S] of DIN 53160-1-2002 commodity colour fastness with the hydrochloric acid solution that mass percent concentration is 1 %.
D, test solution 4 (pH 7.58): test solution ultrapure water (tertiary effluent) preparation, often liter of phosphoric acid disodium hydrogen (Na
2hPO
4) 0.260 g, sodium chloride (NaCl) 0.700 g, potassium rhodanide (KSCN) 0.330 g, potassium dihydrogen phosphate (KH
2pO
4) 0.200 g, sodium bicarbonate (NaHCO
3) 1.500 g, potassium chloride (KCl) 1.200 g, see GB/T 16886.15-2003/ISO 10993-15:2000 medicine equipment biological evaluation [S].
E, test solution 5 (pH 8.60): test solution ultrapure water (tertiary effluent) preparation, often liter containing sodium bicarbonate (NaHCO
3) 4.2 g, sodium chloride (NaCl) 0.5 g, sal tartari (K
2cO
3) 0.2 g. imports and exports saliva of textile colour fastness experimental technique [S] see SN/T 1058 – 2002.
4 prepare detection sample according to testing program
According to testing program (table 4), randomly draw the dixie cup 45 of same brand and specification, under cutting out apart from mm place, rim of a cup edge 15, corresponding mouth touches portion of material as test material respectively, amounts to 45.Every 9 is 1 group, totally 5 groups.Calculate the area of every bar test material, and touch area (0.33 dm as the mouth of each dixie cup
2/ pcs).
1 analogizes 9] cause.Different saliva analogies touch the impact of part phthalate ester migration amount each constituent concentration of getting on paper cup rim is phthalic ester mixed standard solution (each composition of phthalate ester is in table 1) 1 mL of 20 μ g/mL in 5 250 mL conical flasks, volatilizees completely to solvent hexane with nitrogen purging.Saliva analogies 150 mL(touches portion of material and saliva analogies area-volume ratio 1 dm by paper cup rim is injected again in each conical flask
2/ 50 mL, convert with it with the area of 9 test materials and obtain testing the saliva analogies volume that add), and be placed in constant temperature oscillator balanced oscillations to 37 DEG C ± 1 DEG C.Then, cut 9 test materials are placed in the good saliva analogies of constant temperature, and are again placed in by conical flask in constant temperature oscillator (temperature: 37 DEG C ± 1 DEG C, oscillation frequency: 80 r/min), vibrate 30 min ± 1 min.
After vibration terminates, saliva analogies extract is transferred to while hot sealing in conical flask to preserve.After liquid to be extracted gets back to room temperature, accurately measure be equivalent to 3 paper cup rims touch part extract 50 mL in 125 mL separating funnels, and add benzoic acid Bian ester (interior mark) solution 1 mL of 0.5 mg/L, extract 3 times (each 30 mL) with chromatographic pure dichloromethane.Merge organic phase, add a small amount of anhydrous sodium sulfate drying and spend the night.Concentrate organic phase near dry with Rotary Evaporators, then it is to be detected to be settled to 1 mL with normal hexane.
Each test repeats 3 times altogether in the same way, simultaneously each test system 1 blank sample, and the difference of blank sample and test specimen does not add phthalic ester mixed standard solution in blank sample system.
5 employing pulse Splitless injecting samples, GC-MS test paper rim of a cup touch phthalate ester migration amount in portion of material
Use pulse Splitless injecting samples, GC-MS detects
[16]the amount of phthalate ester in made sample, and with this represent test for each time survey paper cup rim touch phthalate ester migration amount in portion of material, the results are shown in Table 5.Because often kind of test repeats 3 times altogether by scheme, obtain 3 samples, each sample duplicate detection 2 times again, therefore adopt different saliva analogies can obtain 6 different data for different phthalate esters, 6 data do one group, and often organizing data is exactly a sample.As, adopt saliva analogies 1(test solution 1) detect for DMP and obtain 6 different data, these 6 data are sample 1; Adopt saliva analogies 2(test solution 2) detect for DMP and obtain 6 different data, these 6 data are sample 2, by that analogy.
Table 5 paper cup rim touches PAEs migration amount in portion of material (μ g/3 pcs)
f
F, 18 kinds of phthalate ester isoconcentrations contained by the mixed standard solution that this test uses, and the detectability of diisononyl phthalate (DINP) and diisooctyl phthalate (DIDP) is than detection limit for height 1 order of magnitude of other phthalate material, therefore fail to detect acquisition diisononyl phthalate (DINP) and diisooctyl phthalate (DIDP) related data.In addition, because DCHP and DNOP data variance is uneven, do not list at this.
6 pairs are detected data and carry out homogeneity test of variance
In order to the difference section changed by saliva analogies between test findings that difference between the test findings that causes and error cause separates, variance analysis or approximating variances analysis can be carried out to test findings (table 5)
[17,18].To homogeneity test of variance be carried out before variance analysis, the results are shown in Table 6.
Table 6 homogeneity test of variance result table
G, in homogeneity test of variance result, if Sig. >=0.05, differentiates that variance is neat; If Sig. < 0.05, differentiate heterogeneity of variance.
7 adopt Welch and Brown-Forsythe two kinds of methods to carry out approximating variances analysis, F significance test to detection data
[17,18]
Table 6 shows, select different saliva analogies, each sample variance is inconsistent, i.e. heterogeneity of variance.Now, existing Welch and Brown-Forsythe two kinds of methods are adopted
[17,18]calculate F value and degree of freedom corrected value, and the practical significant probability of F value through overcorrect.Based on the approximating variances analysis result of heterogeneity of variance in table 7.
Table 7 is based on the approximating variances analysis result of heterogeneity of variance
H, asymptotic F distribution.
I, if Sig. > 0.05, differentiates that saliva analogies are not remarkable on the impact of PAEs migration amount; If Sig. < 0.05, differentiate that saliva analogies are on the impact of PAEs migration amount significantly.
Can judge according to table 7 approximating variances analysis result: saliva analogies have appreciable impact to DMP, DEP, DIBP, DBP, DMEP, BMPP, DEEP, DPP, DHXP, DEHP, DNP migration amount and PAEs gross migration.
8 Multiple range test
Owing to only can infer that according to approximating variances analysis result 5 kinds of saliva analogies touch phthalate ester migration amount in portion of material to paper cup rim and affect whether there were significant differences.If whether there were significant differences to need to touch phthalate ester migration amount impact in portion of material to paper cup rim between deduction 5 kinds of saliva analogies, just need to compare between two average, i.e. Multiple range test.
During heterogeneity of variance, 4 kinds of methods such as conventional Multiple range test method mainly contains Tamhane, Dunnett T3, Games-Howell and Dunnett C
[15,17,18].Closely, test effect is basically identical for the average significance of difference probability that these 4 kinds of methods calculate.Because phthalate ester homolog is more, its Multiple range test data volume is comparatively large, only lists different saliva analogies touch phthalate ester gross migration impact in portion of material the result of multiple comparisons (table 8) on paper cup rim here for this reason.
The different saliva analogies of table 8 touch the result of multiple comparisons of phthalate ester gross migration impact in portion of material to paper cup rim
J, *, represent that between two class means that these data are corresponding, there were significant differences, the significance probability Sig. < 0.05. of its correspondence
Table 8 shows, saliva analogies 3(pH=6.80) paper cup rim is touched to phthalate ester gross migration in portion of material impact and other 4 kinds of saliva analogies compared with there were significant differences, and between other 4 kinds of saliva analogies, significant difference be there is no on the impact that paper cup rim touches phthalate ester gross migration in portion of material.
9 draw Average value compare figure
[15,17,18]
Touch phthalate ester migration amount average in portion of material according to the paper cup rim of each sample, draw Average value compare figure (Fig. 1 ~ Figure 15).Can find out that different saliva analogies touch the affecting laws of phthalate ester migration amount portion of material to paper cup rim intuitively from Average value compare figure.
10 determine to measure the best saliva analogies that paper cup rim touches phthalate ester migration amount in portion of material
In conjunction with the result of multiple comparisons (table 8) and Average value compare figure (Fig. 1 ~ Figure 15), can judge: compared with other 4 kinds of saliva analogies, adopt saliva analogies 3(test solution 3, pH=6.80) measure paper cup rim and touch phthalate ester migration amount in portion of material, its numerical value is minimum.For protecting consumers in general to greatest extent, when analyzing paper cup rim and touching phthalate ester in portion of material to the migration amount in oral cavity, reality to be simulated as far as possible and allowing migration amount maximum (hoping large).Therefore, the saliva analogies touching phthalate ester migration amount in portion of material in order to measure paper cup rim had better not use test solution 3, can adopt test solution 4(pH 7.58): often liter of ultrapure water (tertiary effluent) phosphoric acid disodium hydrogen (Na
2hPO
4) 0.260 g, sodium chloride (NaCl) 0.700 g, potassium rhodanide (KSCN) 0.330 g, potassium dihydrogen phosphate (KH
2pO
4) 0.200 g, sodium bicarbonate (NaHCO
3) 1.500 g, potassium chloride (KCl) 1.200 g (see GB/T 16886.15-2003/ISO 10993-15:2000 medicine equipment biological evaluation [S]).
Claims (1)
1. screen and affect the method that paper cup rim touches the saliva analogies of material phthalate ester migration amount, it is characterized in that the step of the method is as follows:
(1) determine that test index is the migration amount that paper cup rim touches phthalate ester in portion of material, unit is μ g/3 pcs;
(2) test factor and level thereof is determined: test factor is defined as saliva analogies kind, and level is 5 levels, is respectively
pH 2.50 test solution, with ultrapure water preparation, often liter of sodium chloride-containing 4.5 g, potassium chloride 0.3 g, sodium sulphate 0.3 g, ammonium chloride 0.4 g, lactic acid 3.0 g, urea 0.2 g;
pH 6.40 test solution, ultrapure water;
pH 6.80 test solution, test solution ultrapure water is prepared, often liter containing Magnesium dichloride hexahydrate 0.17 g, CALCIUM CHLORIDE DIHYDRATE 0.15 g, two hypophosphite monohydrate hydrogen dipotassium 0.76 g, sal tartari 0.53 g, sodium chloride 0.33 g, potassium chloride 0.75 g, regulates pH to 6.80 ± 0.1 with the hydrochloric acid solution that mass percent concentration is 1 %;
pH 7.58 test solution, test solution ultrapure water is prepared, often liter of phosphoric acid disodium hydrogen 0.260 g, sodium chloride 0.700 g, potassium rhodanide 0.330 g, potassium dihydrogen phosphate 0.200 g, sodium bicarbonate 1.500 g, potassium chloride 1.200 g;
pH 8.60 test solution, test solution ultrapure water is prepared, and often liter containing sodium bicarbonate 4.2 g, sodium chloride 0.5 g, sal tartari 0.2 g;
(3) select single-factor Random Design to work out testing program, wherein single-factor is the saliva analogies kind that step (2) defines, and area-volume ratio that paper cup rim touches portion of material and saliva analogies is fixed as 1 dm
2/ 50 mL, open-assembly time is fixed as 30 min ± 1 min, and Exposure Temperature is fixed as 37 DEG C ± 1 DEG C;
(4) detection sample is prepared according to testing program;
(5) adopt pulse Splitless injecting samples, migration amount that GC-MS test paper rim of a cup touches phthalate ester in portion of material;
(6) homogeneity test of variance is carried out to detection data;
(7) if sample variance is uneven, Welch and Brown-Forsythe two kinds of methods are adopted to carry out approximating variances analysis, F significance test to detection data;
(8) on the test index having appreciable impact, adopt Tamhane, Dunnett T3, Games-Howell and Dunnett C checks 4 kinds of methods to carry out Multiple range test to detection data;
(9) differentiate that different saliva analogies touch the influence degree of phthalate ester migration amount in portion of material to paper cup rim according to analysis result;
(10) touch phthalate ester migration amount average in portion of material according to the paper cup rim of each sample, draw Average value compare figure, and paper cup rim is touched to the effect tendency of phthalate ester migration amount in portion of material according to Average value compare figure intuitive analysis different saliva analogies;
(11) determine to measure the best saliva analogies that paper cup rim touches phthalate ester migration amount in portion of material.
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| CN101493440B (en) * | 2008-08-06 | 2012-01-04 | 通标标准技术服务（天津）有限公司 | Method for measuring migration volume of phthalic ester and di(2-ethylhexyl) adipate in fatty foodstuff contact material |
| CN102507862B (en) * | 2011-10-16 | 2014-06-18 | 云南烟草科学研究院 | Method for judging degree of influence of cigarette additive concentration on special smoke index |
| CN102520091B (en) * | 2011-12-20 | 2014-07-23 | 中国科学院上海有机化学研究所 | Method for detecting plasticizer content in solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry |
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