聚碳酸酯包装材料中双酚A迁移研究
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摘要
随着我国食品安全问题的频发,食品质量安全已经引起人们的高度重视,食品包装安全是食品安全一个重要的环节,食品包装材料的污染来自于制造过程中的劣质材质及原材料选用,食品是一个复杂的基质,其中含有的糖、酸、盐、油等与包装容器接触,会引起包装物的物理和化学的变化,这些反应导致包装物中有害物质迁移到食品中,造成食品污染。
塑料作为一种合成高分子聚合物是目前增长速度最快的食品包装材料之一,聚碳酸酯(polycarbonate, PC)塑料由于其韧性好、透明度高、耐热等特点广泛用于生产碟子、厨房用品、咖啡机、过滤器、婴儿奶瓶、水瓶等,双酚A (Bisphenol A, BPA)是合成PC的重要单体化合物,可以从PC塑料迁移到食品中,影响人体健康。本文以PC塑料为主要研究对象,采用液相色谱-荧光检测法检测PC塑料中双酚A的迁移量,研究各种外界条件如温度、时间、加热方式等对双酚A向不同pH值和硬度的水溶液、酸、糖等溶液中迁移特性的影响,通过原子力显微镜观察塑料表面形貌变化来表征双酚A迁移的微观特点,深入探索PC材料中双酚A的迁移。研究结果表明：
(1)以二氯甲烷溶解PC水桶和PC奶瓶,利用气相色谱-质谱联用仪分别对溶出的化学物进行分析,PC塑料中的主要污染物为烷烃、酯类、酚类物质,酚类中以双酚A的含量最高,通过高效液相色谱-荧光检测法测定市售PC样品中双酚A的含量,范围在3.24～9.1Omg/kg,可见,PC容器中双酚A的污染较普遍。
(2)通过对PC塑料中双酚A向蒸馏水、15%乙醇、65%乙醇和95%乙醇溶液的迁移量的测定,研究其在醇类物质中的迁移特性,结果表明,双酚A向乙醇溶液中的迁移率受乙醇浓度、温度和时间的影响,不同浓度乙醇溶液中的迁移率大小为：95%乙醇>65%乙醇>15%乙醇>蒸馏水。相同浓度乙醇溶液中,在20～75℃范围内,双酚A迁移率随着接触温度的升高而增加,扩散系数随着温度和乙醇浓度的升高而增加,试验测得扩散系数值比通用扩散系数模型预测值大。
(3)考察了pH值和加热方式对双酚A迁移过程的影响,结果表明,冰乙酸和NaOH,柠檬酸-柠檬酸钠来调节pH值的水溶液,pH>7时,双酚A的迁移量显著增加(P<0.05),说明碱性条件有利于PC材料中双酚A的溶出,通过原子力显微镜观察,经过碱液浸泡后,塑料表面粗糙度变大,表面层的暴露面积增加,使双酚A更容易溶出。微波加热过程中双酚A向自来水、矿泉水和蒸馏水中的迁移量存在显著性差异(P<0.05),恒温加热过程中,矿泉水和自来水中双酚A的迁移量无显著性差异(P>0.05),微波加热比常规恒温加热达迁移平衡的时间缩短近12倍。
(4)研究了不同温度条件下,PC材料中双酚A向盐、糖、酸溶液的迁移,结果表明,在盐溶液中,双酚A向二价盐的迁移量要高于一价盐,二价盐中,Ca2+盐大于Mg2+盐,一价盐中,Na+盐大于K+盐,其中NaCl和KCl溶液浓度高于0.1%时与蒸馏水中双酚A的迁移量有显著性差异(P<0.05),而浓度为0.01%的CaCl2和MgCl2溶液与蒸馏水中双酚A的迁移量有显著性差异(P<0.05)。浓度为0.1%～9.0%的醋酸、柠檬酸、酒石酸、苹果酸、乳酸为酸性食品模拟物中,酸种类不同,对双酚A迁移量的影响趋势也不相同,浓度为0.1%的各酸性浸泡液与蒸馏水中双酚A迁移量有显著性差异(P<0.05)。蔗糖、葡萄糖、乳糖和木糖醇为浸泡液时,随着糖浓度的增加,双酚A迁移量随之增加,1.0%的乳糖、2.0%的葡萄糖、2.0%的蔗糖、1.0%的木糖醇与蒸馏水之间双酚A的迁移量存在显著性差异(P<0.05),其中以木糖醇溶液中双酚A的增加幅度最大。
(5)以PC容器盛装茶水和冲调食品作为研究对象,研究温度、时间对双酚A迁出量的影响。结果表明,同种茶叶在95℃加热1h后,双酚A的量在冲调浓度为1.25%、2.0%、5.0%的茶水之间有显著性差异(P<0.05),茶叶种类不同,对双酚A迁移量的影响也不相同,低浓度(1.25%)各茶水之间双酚A的迁移量无显著性差异(P>0.05),而中等浓度(2.0%)的各茶水中双酚A的迁移量存在显著性差异(P<0.05),高浓度茶水(5.0%)中以铁观音中双酚A迁移量最高,茉莉花茶中迁移量最少,毛峰和红茶之间双酚A的迁移量无显著性差异(P>0.05)。温度和食品种类不同导致双酚A的迁移量存在差异,各冲调食品中双酚A迁移量范围在3.44～41.74μg/kg之间,其中以咖啡和奶粉中双酚A的迁移量较多。
With the frequent appearances of food safety problems in China, food quality and safety had drawn great attention of researchers. Food packaging safety is one of the most important parts in food safety. Most pollution of food packaging materials results from the uses of inferior packaging materials and raw materials during manufacturing process. Food is a complex matrix including sugar, acid, salt and oil which could contact with the packaging container. The interactions of the food ingredients and the packaging container will cause the physical and chemical changes of the packaging materials. These reactions result in the migrations of harmful substances from the packaging materials to the food and thus the food is polluted.
Plastic, as a kind of synthetic polymers, is one of the fastest growing food packaging materials recently. Polycarbonate (PC) plastic is widely used in the production of plate, kitchen supplies, coffeemaker, filter, baby bottles and water bottles and so on because of its characteristics such as toughness, high transparency and heat resistance. Bisphenol A (BPA) is an important monomer compound for PC synthesis, but BPA can migrate from PC plastic to the food materials and may play harmful effect on human health. In the present research, the BPA was selected as the main research target and its migration from PC plastic to food materials was investigated by liquid chromatography-fluorescence detection. The effects of different external conditions including temperature, time and heating methods on the migration features of BPA from the PC plastic to acid, sugar and water at different pH and hardness were investigated. The surface morphology of the plastic was observed by atomic force microscopy to further illuminate the microscopic characteristics of the migration of BPA in PC materials. The results showed that:
(1) The PC buckets and PC baby bottles were dissolved by dichloromethane and the dissolved chemical substances were detected by gas chromatograph-mass spectrometer. The main pollutants in the PC plastics are alkanes, esters and phenolic substances and the phenolic substances displayed the highest BPA concentration. The BPA concentrations in the market PC samples ranged from3.24to9.10mg/kg as detected by high performance liquid chromatography-fluorescence. It is revealed that PC containers are commonly polluted by BPA.
(2) The migration amounts of BPA from PC plastics to distilled water and different concentrations of ethanol solutions (15%,65%and95%) were detected to explore its migration features in the alcohols. The results showed that the migration of BPA in ethanol was affected by ethanol concentrations, temperature and time. The migration amounts in different concentrations ethanol were95%ethanol>65%ethanol>15%ethanol> distilled water. In the same ethanol concentration, the migration amounts of BPA increased with the contact temperature increased form20℃to75℃. The diffusion coefficient increased with the increasing temperature and ethanol concentration. The diffusion coefficient value measured in the present experiment is higher than the predicted value by the general diffusion coefficient model.
(3) The effects of pH and heating methods on the migration process of BPA were investigated. The pH of the water was regulated by glacial acetic acid, NaOH, citric acid-sodium citrate. The migration amount of BPA significantly increased above pH7(P<0.05). It is revealed that the alkaline conditions are favorable for the migration of BPA in PC materials. The observations with atomic force microscopy showed that the plastic surface became rougher after soaked by alkali solution. The surface layer is exposed which make bisphenol A easier to dissolution. There is a significant difference in the migration of BPA in tap water, mineral water and distilled water in the microwave heating process (P>0.05). In the constant temperature heating process, there is no significant difference in migration of BPA (P>0.05) between mineral water and tap water. The equilibrium time of the migration by the microwave heating was shortened nearly12times than that by constant temperature heating.
(4) The migration of BPA from PC materials to the salt, sugar and acid solutions at different temperature were investigated. The results showed that the migration of BPA in two valent salt solution was higher than that in the monovalent salt solution. In the two valent salt solution, the migration of BPA was higher in Ca+salt than that in Mg+salt. In the monovalent salt solution, the migration of BPA was higher in Na+salt than that in K+salt. When the NaCl and KCl concentrations were higher than0.1%, the migration amount of BPA in NaCl and KCl solutions were significantly different from that in distilled water (P<0.05). When the CaCl2and MgCl2concentrations were0.01%, the migration amount of BPA in CaCl2and MgCl2solutions were significantly different from that in distilled water (P<0.05). The0.1%-9.0%concentrations of acetic acid, citric acid, tartaric acid, malic acid and lactic acid were selected as acid food simulants. Different types of acids showed different effects on the migration amount of BPA. There is a significant difference of the BPA migration amount between the0.1%acid soaking solution and distilled water (P<0.05). With the increasing concentrations of sucrose, glucose, lactose and xylitol, the migration amount of BPA increased. The migration amounts of BPA in1%lactose,2%glucose,2%sucrose,1%xylitol were significant different from that in distilled water (.P<0.05) and the xylitol solution showed the highest migration amount of BPA.
(5) The effect of temperature and time on the migration amount of BPA in the PC containers containing tea and reconstituted food were investigated. When the same kind of tea at1.25%,2%,5%concentrations were heated at95℃for1h, the BPA amount displayed significant differences at different concentrations of tea (P<0.05). Different types of tea played different roles on the migration of BPA. When the tea level was1.25%, there is no significant difference among different types of tea (P>0.05). When the tea concentration increased to2%, the BPA amount were significantly different among different types of tea (P<0.05). At high concentration (5%), the migration amount of BPA in Tie Guan Yin was the highest, and the jasmine tea showed the least migration amount of BPA. There is no significant difference between the Mao Feng and black tea (P>0.05). Different temperature and food types resulted in different migration amount of BPA. The migration of BPA in different food is in the range of3.44-41.74μg/kg, in which coffee and milk powder showed higher migration amount of BPA.
塑料作为一种合成高分子聚合物是目前增长速度最快的食品包装材料之一,聚碳酸酯(polycarbonate, PC)塑料由于其韧性好、透明度高、耐热等特点广泛用于生产碟子、厨房用品、咖啡机、过滤器、婴儿奶瓶、水瓶等,双酚A (Bisphenol A, BPA)是合成PC的重要单体化合物,可以从PC塑料迁移到食品中,影响人体健康。本文以PC塑料为主要研究对象,采用液相色谱-荧光检测法检测PC塑料中双酚A的迁移量,研究各种外界条件如温度、时间、加热方式等对双酚A向不同pH值和硬度的水溶液、酸、糖等溶液中迁移特性的影响,通过原子力显微镜观察塑料表面形貌变化来表征双酚A迁移的微观特点,深入探索PC材料中双酚A的迁移。研究结果表明：
(1)以二氯甲烷溶解PC水桶和PC奶瓶,利用气相色谱-质谱联用仪分别对溶出的化学物进行分析,PC塑料中的主要污染物为烷烃、酯类、酚类物质,酚类中以双酚A的含量最高,通过高效液相色谱-荧光检测法测定市售PC样品中双酚A的含量,范围在3.24～9.1Omg/kg,可见,PC容器中双酚A的污染较普遍。
(2)通过对PC塑料中双酚A向蒸馏水、15%乙醇、65%乙醇和95%乙醇溶液的迁移量的测定,研究其在醇类物质中的迁移特性,结果表明,双酚A向乙醇溶液中的迁移率受乙醇浓度、温度和时间的影响,不同浓度乙醇溶液中的迁移率大小为：95%乙醇>65%乙醇>15%乙醇>蒸馏水。相同浓度乙醇溶液中,在20～75℃范围内,双酚A迁移率随着接触温度的升高而增加,扩散系数随着温度和乙醇浓度的升高而增加,试验测得扩散系数值比通用扩散系数模型预测值大。
(3)考察了pH值和加热方式对双酚A迁移过程的影响,结果表明,冰乙酸和NaOH,柠檬酸-柠檬酸钠来调节pH值的水溶液,pH>7时,双酚A的迁移量显著增加(P<0.05),说明碱性条件有利于PC材料中双酚A的溶出,通过原子力显微镜观察,经过碱液浸泡后,塑料表面粗糙度变大,表面层的暴露面积增加,使双酚A更容易溶出。微波加热过程中双酚A向自来水、矿泉水和蒸馏水中的迁移量存在显著性差异(P<0.05),恒温加热过程中,矿泉水和自来水中双酚A的迁移量无显著性差异(P>0.05),微波加热比常规恒温加热达迁移平衡的时间缩短近12倍。
(4)研究了不同温度条件下,PC材料中双酚A向盐、糖、酸溶液的迁移,结果表明,在盐溶液中,双酚A向二价盐的迁移量要高于一价盐,二价盐中,Ca2+盐大于Mg2+盐,一价盐中,Na+盐大于K+盐,其中NaCl和KCl溶液浓度高于0.1%时与蒸馏水中双酚A的迁移量有显著性差异(P<0.05),而浓度为0.01%的CaCl2和MgCl2溶液与蒸馏水中双酚A的迁移量有显著性差异(P<0.05)。浓度为0.1%～9.0%的醋酸、柠檬酸、酒石酸、苹果酸、乳酸为酸性食品模拟物中,酸种类不同,对双酚A迁移量的影响趋势也不相同,浓度为0.1%的各酸性浸泡液与蒸馏水中双酚A迁移量有显著性差异(P<0.05)。蔗糖、葡萄糖、乳糖和木糖醇为浸泡液时,随着糖浓度的增加,双酚A迁移量随之增加,1.0%的乳糖、2.0%的葡萄糖、2.0%的蔗糖、1.0%的木糖醇与蒸馏水之间双酚A的迁移量存在显著性差异(P<0.05),其中以木糖醇溶液中双酚A的增加幅度最大。
(5)以PC容器盛装茶水和冲调食品作为研究对象,研究温度、时间对双酚A迁出量的影响。结果表明,同种茶叶在95℃加热1h后,双酚A的量在冲调浓度为1.25%、2.0%、5.0%的茶水之间有显著性差异(P<0.05),茶叶种类不同,对双酚A迁移量的影响也不相同,低浓度(1.25%)各茶水之间双酚A的迁移量无显著性差异(P>0.05),而中等浓度(2.0%)的各茶水中双酚A的迁移量存在显著性差异(P<0.05),高浓度茶水(5.0%)中以铁观音中双酚A迁移量最高,茉莉花茶中迁移量最少,毛峰和红茶之间双酚A的迁移量无显著性差异(P>0.05)。温度和食品种类不同导致双酚A的迁移量存在差异,各冲调食品中双酚A迁移量范围在3.44～41.74μg/kg之间,其中以咖啡和奶粉中双酚A的迁移量较多。
With the frequent appearances of food safety problems in China, food quality and safety had drawn great attention of researchers. Food packaging safety is one of the most important parts in food safety. Most pollution of food packaging materials results from the uses of inferior packaging materials and raw materials during manufacturing process. Food is a complex matrix including sugar, acid, salt and oil which could contact with the packaging container. The interactions of the food ingredients and the packaging container will cause the physical and chemical changes of the packaging materials. These reactions result in the migrations of harmful substances from the packaging materials to the food and thus the food is polluted.
Plastic, as a kind of synthetic polymers, is one of the fastest growing food packaging materials recently. Polycarbonate (PC) plastic is widely used in the production of plate, kitchen supplies, coffeemaker, filter, baby bottles and water bottles and so on because of its characteristics such as toughness, high transparency and heat resistance. Bisphenol A (BPA) is an important monomer compound for PC synthesis, but BPA can migrate from PC plastic to the food materials and may play harmful effect on human health. In the present research, the BPA was selected as the main research target and its migration from PC plastic to food materials was investigated by liquid chromatography-fluorescence detection. The effects of different external conditions including temperature, time and heating methods on the migration features of BPA from the PC plastic to acid, sugar and water at different pH and hardness were investigated. The surface morphology of the plastic was observed by atomic force microscopy to further illuminate the microscopic characteristics of the migration of BPA in PC materials. The results showed that:
(1) The PC buckets and PC baby bottles were dissolved by dichloromethane and the dissolved chemical substances were detected by gas chromatograph-mass spectrometer. The main pollutants in the PC plastics are alkanes, esters and phenolic substances and the phenolic substances displayed the highest BPA concentration. The BPA concentrations in the market PC samples ranged from3.24to9.10mg/kg as detected by high performance liquid chromatography-fluorescence. It is revealed that PC containers are commonly polluted by BPA.
(2) The migration amounts of BPA from PC plastics to distilled water and different concentrations of ethanol solutions (15%,65%and95%) were detected to explore its migration features in the alcohols. The results showed that the migration of BPA in ethanol was affected by ethanol concentrations, temperature and time. The migration amounts in different concentrations ethanol were95%ethanol>65%ethanol>15%ethanol> distilled water. In the same ethanol concentration, the migration amounts of BPA increased with the contact temperature increased form20℃to75℃. The diffusion coefficient increased with the increasing temperature and ethanol concentration. The diffusion coefficient value measured in the present experiment is higher than the predicted value by the general diffusion coefficient model.
(3) The effects of pH and heating methods on the migration process of BPA were investigated. The pH of the water was regulated by glacial acetic acid, NaOH, citric acid-sodium citrate. The migration amount of BPA significantly increased above pH7(P<0.05). It is revealed that the alkaline conditions are favorable for the migration of BPA in PC materials. The observations with atomic force microscopy showed that the plastic surface became rougher after soaked by alkali solution. The surface layer is exposed which make bisphenol A easier to dissolution. There is a significant difference in the migration of BPA in tap water, mineral water and distilled water in the microwave heating process (P>0.05). In the constant temperature heating process, there is no significant difference in migration of BPA (P>0.05) between mineral water and tap water. The equilibrium time of the migration by the microwave heating was shortened nearly12times than that by constant temperature heating.
(4) The migration of BPA from PC materials to the salt, sugar and acid solutions at different temperature were investigated. The results showed that the migration of BPA in two valent salt solution was higher than that in the monovalent salt solution. In the two valent salt solution, the migration of BPA was higher in Ca+salt than that in Mg+salt. In the monovalent salt solution, the migration of BPA was higher in Na+salt than that in K+salt. When the NaCl and KCl concentrations were higher than0.1%, the migration amount of BPA in NaCl and KCl solutions were significantly different from that in distilled water (P<0.05). When the CaCl2and MgCl2concentrations were0.01%, the migration amount of BPA in CaCl2and MgCl2solutions were significantly different from that in distilled water (P<0.05). The0.1%-9.0%concentrations of acetic acid, citric acid, tartaric acid, malic acid and lactic acid were selected as acid food simulants. Different types of acids showed different effects on the migration amount of BPA. There is a significant difference of the BPA migration amount between the0.1%acid soaking solution and distilled water (P<0.05). With the increasing concentrations of sucrose, glucose, lactose and xylitol, the migration amount of BPA increased. The migration amounts of BPA in1%lactose,2%glucose,2%sucrose,1%xylitol were significant different from that in distilled water (.P<0.05) and the xylitol solution showed the highest migration amount of BPA.
(5) The effect of temperature and time on the migration amount of BPA in the PC containers containing tea and reconstituted food were investigated. When the same kind of tea at1.25%,2%,5%concentrations were heated at95℃for1h, the BPA amount displayed significant differences at different concentrations of tea (P<0.05). Different types of tea played different roles on the migration of BPA. When the tea level was1.25%, there is no significant difference among different types of tea (P>0.05). When the tea concentration increased to2%, the BPA amount were significantly different among different types of tea (P<0.05). At high concentration (5%), the migration amount of BPA in Tie Guan Yin was the highest, and the jasmine tea showed the least migration amount of BPA. There is no significant difference between the Mao Feng and black tea (P>0.05). Different temperature and food types resulted in different migration amount of BPA. The migration of BPA in different food is in the range of3.44-41.74μg/kg, in which coffee and milk powder showed higher migration amount of BPA.
引文
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