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Studies On The Determination And Migration Of Phthalate Esters In Edible Oil

Posted on:2012-11-06Degree:MasterType:Thesis
Country:ChinaCandidate:Y C HuFull Text:PDF
GTID:2131330335953118Subject:Food Science
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The use of plasticizers, toxicity of PAEs and migration laws of monomers in such plasticizers under the packaging process at home and abroad are summarized, and some suggestions about strengthening research and management of food package materials are raised through compared the limited standards between China and other major developed countries in this paper.In order to detect the pollution of phthalic acid esters in edible oil, the method for determination of phthalic acid esters from edible oil by GC-MS is researched. The sample was dissolved in cyclohexane-ethylacetate and purified by GPC. Then it measured by GC-MS, using external standard method to quantitative analysis. In the 50~5000μg/L scope, it has the good linear relationship (R2>0.997). Detectable limit is smaller than 40μg/kg. On the add level of 100~5000μg/kg, the recovery rate is in the ranged of 81.52%~99.27%, the relatives standard deviation is in 0.32%~4.73%. The relatives standard deviation of method experimental precision are within 5%.Quantitative results of matrix added standard calibration trace are better than standard preparation calibration trace.The method for determination of phthalic acid esters from edible oil by HPLC is researched. The sample was dissolved in cyclohexane-ethylacetate and purified by GPC. Then it measured by HPLC, using external standard method to quantitative analysis. In the0.1~8.0mg/L scope, it has the good linear relationship (R2>0.9998); lowest detectable limit of analytical method smaller than 50μg/L; lowest detectable limit of instrument smaller than 200μg/kg; the recovery rate of the phthalic acid esters at 0.5μg/mL,1.0μg/mL and 8.0μg/mL addition were ranged from 92.70%~98.84%, the relatively standard deviation is in 1.81%~4.71%. The relatives standard deviation of Sample experimental precision are within 5%. Quantitative results of standard preparation calibration trace are better than matrix added standard calibration trace.The method for determination of it from edible oil by LC/MS/MS is researched. The sample was dissolved in cyclohexane-ethylacetate and purified by GPC. Then it measured by LC/MS/MS, using external standard method to quantitative analysis. In the 50~400μg/L scope, it has the good linear relationship (R2>0.99). Detectable limit is smaller than 35μg/kg. On the add level of 50,200,400μg/kg, the PAEs recovery rate is in the ranged of 90.07%~99.53%, the relatives standard deviation is in 2.21%~4.82%. The relatives standard deviation of method experimental precision are within 5%.Quantitative results of matrix added standard calibration trace are better than standard preparation calibration trace.In oder to accurately detect the content of PAEs in plastic bottle which is used to storage edible oil.The response surface methodology were made on it from plastic bottled by soxhlet extraction.The effect of different extraction solvents, ratio of material to solvent, extraction temperature and extraction time on PAEs extraction were discussed. The Box-Behnken design was applied to fit a response surface function, which based on the one-variable-at-time design. Through the function we can get the optimum extraction conditions, the optimal levels were as follows: the extraction solvents is trichlormethane, the extraction temperature is 63℃, the extraction time is 5h.the ratio of material to solvent is 2:26.4,the PAEs content value is 108.782mg/kg.Migration experiment was designed by design expert. The model of PAEs migrate to edible oil was established. The migration model as follow, Y1=44.48-3.18A- 0.011B+8.49C- 0.096AB-3.98AC-0.34BC-6.03A2-15.548B2-10.71C2-0.21ABC-0.54A~2B-0.29A~2C+0.38AB~2-1.12 AC~2-0.3 B~2C -0.95BC~2-0.93A~3-0.68 B~3-0.47 C~3. The factors order on migration of PAEs as follow, gration temperature, migration time , ratio of solvent to material.The relative error of the model's predictive value is less than 5% by verification experiment.It indicates that the model can accurately predict the migration of PAEs in the edible oil.
Keywords/Search Tags:GC-MS, Phthalic acid esters, Migration model, Plasticizer, HPLC
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