食品级PVC膜中增塑剂邻苯二甲酸二（2-乙基己基）酯迁移特性研究
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摘要
食品包装材料的卫生安全是保障食品安全的重要方面,食品级PVC膜中大量使用邻苯二甲酸酯类增塑剂,其潜在迁移性对人体健康的危害引起了社会的关注。本文以食品级PVC膜为研究对象,研究了增塑剂邻苯二甲酸二(2-乙基己基)酯(DEHP)向食品中的迁移特性。本文首先研究了PVC膜中增塑剂DEHP向各类食品模拟液中的迁移,然后,建立了猪肉中DEHP的气相色谱检测方法,研究了温度、时间、脂肪含量、pH值等因素对PVC膜中增塑剂DEHP向猪肉中迁移的影响,随后探讨了微波、紫外照射作用下,PVC膜中增塑剂DEHP向食品中的迁移,最后分析了煮、炸等烹饪方式对肉中DEHP存留量变化的影响。本论文得出的主要结论有:
1、建立了常用食品塑料包装材料中增塑剂DEHP的气相色谱检测方法。选用乙醚为提取溶剂,索氏提取4h,该方法回收率为90.7～105.1%,检出限为6.76×10-4μg/mL,折合成样品中的检出限为3.38×10-3mg/kg。
2、PVC膜中DEHP能迁移到水性食品模拟液中。(1)相对于乙醚、正己烷,三氯甲烷是萃取水性食品模拟液中迁移的DEHP的最好溶剂;(2)DEHP在水性食品模拟液中迁移率大小为:65%乙醇>20%乙醇>蒸馏水>4%乙酸;(3)不同浸泡条件下,DEHP的迁移率范围为0.19%～0.38%(蒸馏水)、0.19%～0.45%(20%乙醇)、0.72%～6.32%(65%乙醇)。
3、建立了猪肉中DEHP的皂化蒸馏检测方法。该方法的工艺参数为:用乙醚提取6h,皂化3h,使DEHP分解为邻苯二甲酸和2-乙基-1-己醇,用水蒸气蒸馏出2-乙基-1-己醇,通过测定2-乙基-1-己醇的含量,换算出DEHP含量。该方法加标回收率为75.12%～84.95%,检出限为1.07×10-3mg/kg。
4、温度、时间、脂肪含量、pH值会影响PVC膜中增塑剂DEHP向猪肉中的迁移量。(1)DEHP向猪肉中的迁移量随接触时间的延长、温度的升高而增加,温度90℃、接触0.5h的迁移量为1961.92mg/kg(75.12mg/dm2);(2)脂肪含量越高,DEHP迁移量越大。膜/肉接触60h后,脂肪含量45.2%的肉样中DEHP迁移量达到了2255.91mg/kg(55.68mg/dm2,20℃);(3)肉样不腐败变质的情况下,pH为6前后,样品中增塑剂的迁移量最大,最高值为1281.59mg/kg(49.00mg/dm2,膜/肉接触48h,20℃)。
5、紫外、微波作用能够增加PVC膜中增塑剂DEHP向猪肉中的迁移量。(1)与未照射样品比较,紫外照射12h迁移量增加39.55%;(2)微波功率850W,辐射16s,平均迁移量为534.92mg/kg(13.76mg/dm2),而未辐射对照样品DEHP未检出。
6、污染样品煮制、炸制后,样品中DEHP的含量显著降低。(1)煮制30min后,样品中DEHP含量下降了50.96%,从536.80mg/kg下降到263.26mg/kg;(2)炸制3min后,样品中DEHP含量下降了61.49%,从536.80mg/kg下降到206.70mg/kg。
7、DEHP向各类食品中的迁移量不同。(1)皂化蒸馏测定方法应用于高脂肪食品中DEHP的检测时,DEHP的回收率在56.39%～97.40%之间;(2)膜/肉接触24h(20℃)后,16份样品中,DEHP的检出率为68.75%。检出DEHP的样品中,迁移量范围为635.97mg/kg(17.71mg/dm2)～892.03mg/kg(25.58mg/dm2)。
8、本研究的创新点在于:(1)首次建立了猪肉中DEHP的皂化蒸馏检测方法;(2)建立了索氏提取气相色谱DEHP测定方法;(3)首次运用膜/肉接触的比色管模式,成功研究了PVC膜/肉接触时,温度、时间、脂肪含量、pH值对增塑剂DEHP向猪肉中迁移的迁移量的影响。
本研究为PVC膜中增塑剂DEHP向食品中的迁移问题,提供了廉价、快速的检测方法,给出了DEHP在不同接触条件下的迁移量,为保障食品包装的安全提供了有力工具。
The safety and sanitation of food plastic packaging materials are important aspects of ensuring food safety. Plasticizer PAEs are widely used in food grade PVC film and the jeopardize of migration arousing people’s attention. This paper studies the migration of Di-2-ethylhexyl phthalate (DEHP) existing in food grade PVC film. Firstly, migration of DEHP from food grade PVC film into water food simulants was studied; secondly, GC method of determining DEHP in meat was established; thirdly, the influence of temperature, time, fat content and pH on the migration of DEHP into meat was investigated; fourthly, migration of DEHP under UV radiation and microwave was worked over, lastly, the influence of cooking and frying on DEHP content in meat was studied. The paper affords major results as follows:
1. The determining method of DEHP in food plastic packaging materials was established by GC. The results showed that solvent was diethyl ether, soxhlet extracting 4h, the recovery rate lied between 90.7% and 105.1% and the detection limit was 6.76×10-4μg/ml in solution and 3.38×10-3mg/kg in sample.
2. DEHP could migrate into all water food simulants from PVC film. (1) Trichloromethane was the best extracting solvent of DEHP in water food simulants compared with diethyl ether and hexane; (2) The sequence of DEHP migration rate in water food simulants was: 65% ethanol>20% ethanol>water>4% acetic acid; (3) Under different circumstances, range of DEHP migration rate was 0.19%～0.38%(water), 0.19%～0.45%(20% ethanol), 0.72%～6.32%(65% ethanol), respectively.
3. The determining method of DEHP in meat was established by saponification and distillation. The technologic parameters were: extracted 6h by diethyl ether firstly, saponified 3h secondly, thus DEHP decomposed to phthalic acid and 2-ethyl-1-hexanol. 2-Ethyl-1-hexanol was determined after being steam distilled and the amount of DEHP was calculated by conversion. The recovery rate of the method lied between 75.12% and 84.95%, detection limit was 1.07×10-3mg/kg.
4. Amount of migration of DEHP from PVC film into meat was influenced by temperature, time, fat content and pH value. (1) Amount of migration of DEHP increased with the time prolonging and temperature increasing. The amount of migration of DEHP was 1961.92mg/kg (75.12mg/dm2, 90℃, film/meat contacting 0.5h); (2). Amount of migration of DEHP increased with fat content adding. After film/meat contacting 60h, the amount of migration of DEHP in 45.2% samples reached 2255.91mg/kg (55.68mg/dm2, 20℃); (3) The amount of migration of DEHP was the highest in pH6 samples before meat degenerative and the top value was 1281.59 mg/kg (49.00mg/dm2, film/meat contacting 48h, 20℃).
5. Ultraviolet radiation and microwave could enhance the migration of DEHP from PVC film into meat. (1) After Ultraviolet radiating 12h, the amount of migration of DEHP was 39.55% higher than control samples; (2) The average amount of migration of DEHP was 534.92mg/kg (13.76mg/dm2) after microwave heating 16s, 850W, while the control samples under detection.
6. The amount of DEHP in contaminated samples significantly decreased after cooking and frying. (1) After cooking 30min, the amount of DEHP was lower 50.96%, from 536.80mg/kg to 263.26mg/kg before and after cooking; (2) After frying 3min, the amount of DEHP was lower 61.49%, from 536.80mg/kg to 206.70mg/kg before and after frying.
7. Amount of migration of DEHP differed in different foods. (1) The recovery rate of DEHP saponification and distillation method ranged from 56.39% to 97.40% in different foods; (2) The picks out rate of DEHP was 68.75% in 16 samples after film/meat contacting 24h(20℃) . The range of amount of migration of DEHP was 635.97mg/kg (17.71mg/dm2)～892.03mg/kg (25.58mg/dm2) in picked out samples.
8. The innovation of the paper was as follows: (1) The determining method of DEHP in meat was established by saponification and distillation for the first time; (2) The determining method of DEHP in food plastic packaging materials was established by GC and soxhlet extracted; (3) The influence of temperature, time, fat content and pH on the migration of DEHP from PVC film into meat was successfully researched by using the model of Colorimetric tube of film/meat contacting for the first time.
The paper affords cheap and rapid determining methods and amount of migration of DEHP under different contacting conditions for researching the migration of DEHP from food grade PVC film into foods and offers strongly instrument for ensuring the safety of food packaging.
1、建立了常用食品塑料包装材料中增塑剂DEHP的气相色谱检测方法。选用乙醚为提取溶剂,索氏提取4h,该方法回收率为90.7～105.1%,检出限为6.76×10-4μg/mL,折合成样品中的检出限为3.38×10-3mg/kg。
2、PVC膜中DEHP能迁移到水性食品模拟液中。(1)相对于乙醚、正己烷,三氯甲烷是萃取水性食品模拟液中迁移的DEHP的最好溶剂;(2)DEHP在水性食品模拟液中迁移率大小为:65%乙醇>20%乙醇>蒸馏水>4%乙酸;(3)不同浸泡条件下,DEHP的迁移率范围为0.19%～0.38%(蒸馏水)、0.19%～0.45%(20%乙醇)、0.72%～6.32%(65%乙醇)。
3、建立了猪肉中DEHP的皂化蒸馏检测方法。该方法的工艺参数为:用乙醚提取6h,皂化3h,使DEHP分解为邻苯二甲酸和2-乙基-1-己醇,用水蒸气蒸馏出2-乙基-1-己醇,通过测定2-乙基-1-己醇的含量,换算出DEHP含量。该方法加标回收率为75.12%～84.95%,检出限为1.07×10-3mg/kg。
4、温度、时间、脂肪含量、pH值会影响PVC膜中增塑剂DEHP向猪肉中的迁移量。(1)DEHP向猪肉中的迁移量随接触时间的延长、温度的升高而增加,温度90℃、接触0.5h的迁移量为1961.92mg/kg(75.12mg/dm2);(2)脂肪含量越高,DEHP迁移量越大。膜/肉接触60h后,脂肪含量45.2%的肉样中DEHP迁移量达到了2255.91mg/kg(55.68mg/dm2,20℃);(3)肉样不腐败变质的情况下,pH为6前后,样品中增塑剂的迁移量最大,最高值为1281.59mg/kg(49.00mg/dm2,膜/肉接触48h,20℃)。
5、紫外、微波作用能够增加PVC膜中增塑剂DEHP向猪肉中的迁移量。(1)与未照射样品比较,紫外照射12h迁移量增加39.55%;(2)微波功率850W,辐射16s,平均迁移量为534.92mg/kg(13.76mg/dm2),而未辐射对照样品DEHP未检出。
6、污染样品煮制、炸制后,样品中DEHP的含量显著降低。(1)煮制30min后,样品中DEHP含量下降了50.96%,从536.80mg/kg下降到263.26mg/kg;(2)炸制3min后,样品中DEHP含量下降了61.49%,从536.80mg/kg下降到206.70mg/kg。
7、DEHP向各类食品中的迁移量不同。(1)皂化蒸馏测定方法应用于高脂肪食品中DEHP的检测时,DEHP的回收率在56.39%～97.40%之间;(2)膜/肉接触24h(20℃)后,16份样品中,DEHP的检出率为68.75%。检出DEHP的样品中,迁移量范围为635.97mg/kg(17.71mg/dm2)～892.03mg/kg(25.58mg/dm2)。
8、本研究的创新点在于:(1)首次建立了猪肉中DEHP的皂化蒸馏检测方法;(2)建立了索氏提取气相色谱DEHP测定方法;(3)首次运用膜/肉接触的比色管模式,成功研究了PVC膜/肉接触时,温度、时间、脂肪含量、pH值对增塑剂DEHP向猪肉中迁移的迁移量的影响。
本研究为PVC膜中增塑剂DEHP向食品中的迁移问题,提供了廉价、快速的检测方法,给出了DEHP在不同接触条件下的迁移量,为保障食品包装的安全提供了有力工具。
The safety and sanitation of food plastic packaging materials are important aspects of ensuring food safety. Plasticizer PAEs are widely used in food grade PVC film and the jeopardize of migration arousing people’s attention. This paper studies the migration of Di-2-ethylhexyl phthalate (DEHP) existing in food grade PVC film. Firstly, migration of DEHP from food grade PVC film into water food simulants was studied; secondly, GC method of determining DEHP in meat was established; thirdly, the influence of temperature, time, fat content and pH on the migration of DEHP into meat was investigated; fourthly, migration of DEHP under UV radiation and microwave was worked over, lastly, the influence of cooking and frying on DEHP content in meat was studied. The paper affords major results as follows:
1. The determining method of DEHP in food plastic packaging materials was established by GC. The results showed that solvent was diethyl ether, soxhlet extracting 4h, the recovery rate lied between 90.7% and 105.1% and the detection limit was 6.76×10-4μg/ml in solution and 3.38×10-3mg/kg in sample.
2. DEHP could migrate into all water food simulants from PVC film. (1) Trichloromethane was the best extracting solvent of DEHP in water food simulants compared with diethyl ether and hexane; (2) The sequence of DEHP migration rate in water food simulants was: 65% ethanol>20% ethanol>water>4% acetic acid; (3) Under different circumstances, range of DEHP migration rate was 0.19%～0.38%(water), 0.19%～0.45%(20% ethanol), 0.72%～6.32%(65% ethanol), respectively.
3. The determining method of DEHP in meat was established by saponification and distillation. The technologic parameters were: extracted 6h by diethyl ether firstly, saponified 3h secondly, thus DEHP decomposed to phthalic acid and 2-ethyl-1-hexanol. 2-Ethyl-1-hexanol was determined after being steam distilled and the amount of DEHP was calculated by conversion. The recovery rate of the method lied between 75.12% and 84.95%, detection limit was 1.07×10-3mg/kg.
4. Amount of migration of DEHP from PVC film into meat was influenced by temperature, time, fat content and pH value. (1) Amount of migration of DEHP increased with the time prolonging and temperature increasing. The amount of migration of DEHP was 1961.92mg/kg (75.12mg/dm2, 90℃, film/meat contacting 0.5h); (2). Amount of migration of DEHP increased with fat content adding. After film/meat contacting 60h, the amount of migration of DEHP in 45.2% samples reached 2255.91mg/kg (55.68mg/dm2, 20℃); (3) The amount of migration of DEHP was the highest in pH6 samples before meat degenerative and the top value was 1281.59 mg/kg (49.00mg/dm2, film/meat contacting 48h, 20℃).
5. Ultraviolet radiation and microwave could enhance the migration of DEHP from PVC film into meat. (1) After Ultraviolet radiating 12h, the amount of migration of DEHP was 39.55% higher than control samples; (2) The average amount of migration of DEHP was 534.92mg/kg (13.76mg/dm2) after microwave heating 16s, 850W, while the control samples under detection.
6. The amount of DEHP in contaminated samples significantly decreased after cooking and frying. (1) After cooking 30min, the amount of DEHP was lower 50.96%, from 536.80mg/kg to 263.26mg/kg before and after cooking; (2) After frying 3min, the amount of DEHP was lower 61.49%, from 536.80mg/kg to 206.70mg/kg before and after frying.
7. Amount of migration of DEHP differed in different foods. (1) The recovery rate of DEHP saponification and distillation method ranged from 56.39% to 97.40% in different foods; (2) The picks out rate of DEHP was 68.75% in 16 samples after film/meat contacting 24h(20℃) . The range of amount of migration of DEHP was 635.97mg/kg (17.71mg/dm2)～892.03mg/kg (25.58mg/dm2) in picked out samples.
8. The innovation of the paper was as follows: (1) The determining method of DEHP in meat was established by saponification and distillation for the first time; (2) The determining method of DEHP in food plastic packaging materials was established by GC and soxhlet extracted; (3) The influence of temperature, time, fat content and pH on the migration of DEHP from PVC film into meat was successfully researched by using the model of Colorimetric tube of film/meat contacting for the first time.
The paper affords cheap and rapid determining methods and amount of migration of DEHP under different contacting conditions for researching the migration of DEHP from food grade PVC film into foods and offers strongly instrument for ensuring the safety of food packaging.
引文
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