气相色谱法测定塑料食品包装材料在橄榄油中的总迁移量
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摘要
选择聚丙烯(PP)、聚氯乙烯(PVC)及聚乙烯(PE)材质的食品包装材料作为样品,在作为食品模拟物的橄榄油中浸泡一定时间,令样品中的化学物质向食品迁移。样品在橄榄油中浸泡前后均须在干燥器中放置24h,取出后立即称量其质量m_1(浸泡前)及m_2(浸泡后)。用正戊烷作为提取溶剂,用自动索氏提取仪提取吸附在样品上的橄榄油,经皂化-甲酯化获得其甲基酯化产物,用气相色谱内标法测得所有生成的酯化产物的峰面积及其加和总面积。并计算此总峰面积与内标峰面积的比值,从标准曲线上查得其相当于吸附在样品上的橄榄油的质量m_4。由于所测定3种塑料的挥发性损失质量均<2.0mg,不需作质量校正,因而根据[m_1-(m_2-m_4)]的值以及样品与食品接触部位的表面积(dm~2),即可算出样品在橄榄油中的总迁移量M,mg·dm~(-2)。应用此方法检测了几十批样品,除PVC旋开盖外,其他样品的总迁移量均低于规定限量。但由于PVC旋开盖的提取物酯化产物的色谱峰与橄榄油酯化产物的色谱峰的保留时间相同,有严重干扰,故橄榄油不适宜于检测PVC旋开盖。
Three kinds of plastics,i.e.,polypropene(PP),polyvinylchloride(PVC)and polyethylene(PE),commonly used in making food-packaging utensils,were chosen as samples and olive oil was taken as simulant for foodstuffs.The sample was soaked in olive oil for a definite time,during which the chemical substances of the plastic material might have migrated into the simulant.Before and after soaking of the sample in olive oil,the sample was kept in a desiccator for 24 h,and its mass,m_1(before soaking)and m_2(after soaking)was weighed as soon as taking out it from the desiccator.n-Pentane was used as solvent to extract the olive oil adhered on the sample by a automatic soxhlet extractor,and it was determined by GC(with internal standard method)after saponification and methyl-esterification of the adhered olive oil.Values of peak areas of all the methyl esters producted during esterification were taken and sumed up.Ratio of the total peak area to the peak area of internal standard was calculated and the amount of olive oil adhered to the sample(m_4)was found from the standard curve.As the 3 plastic materials concerned,loss of mass due to volatile matter were all less than 2.0 mg,hence correction for loss of mass was not necessary.Then overall migration M(mg·dm~(-2))can be found by the formula given based on the data of[m_1-(m_2-m_4)]and surface area of the sample in contact with the simulated foodstuff(dm~2).The proposed method has been used for determination of overall migration in tens of samples,all the results of Mfound were below the required limit value,beside the results of samples of PVC screw covers.It was found that the esterification products of extract from PVC material gave chromatographic peak nearly same as those of olive oil,leading to significant positive error.Therefore,olive oil can not be use as simulated foodstuff for PVC screw cover.
Three kinds of plastics,i.e.,polypropene(PP),polyvinylchloride(PVC)and polyethylene(PE),commonly used in making food-packaging utensils,were chosen as samples and olive oil was taken as simulant for foodstuffs.The sample was soaked in olive oil for a definite time,during which the chemical substances of the plastic material might have migrated into the simulant.Before and after soaking of the sample in olive oil,the sample was kept in a desiccator for 24 h,and its mass,m_1(before soaking)and m_2(after soaking)was weighed as soon as taking out it from the desiccator.n-Pentane was used as solvent to extract the olive oil adhered on the sample by a automatic soxhlet extractor,and it was determined by GC(with internal standard method)after saponification and methyl-esterification of the adhered olive oil.Values of peak areas of all the methyl esters producted during esterification were taken and sumed up.Ratio of the total peak area to the peak area of internal standard was calculated and the amount of olive oil adhered to the sample(m_4)was found from the standard curve.As the 3 plastic materials concerned,loss of mass due to volatile matter were all less than 2.0 mg,hence correction for loss of mass was not necessary.Then overall migration M(mg·dm~(-2))can be found by the formula given based on the data of[m_1-(m_2-m_4)]and surface area of the sample in contact with the simulated foodstuff(dm~2).The proposed method has been used for determination of overall migration in tens of samples,all the results of Mfound were below the required limit value,beside the results of samples of PVC screw covers.It was found that the esterification products of extract from PVC material gave chromatographic peak nearly same as those of olive oil,leading to significant positive error.Therefore,olive oil can not be use as simulated foodstuff for PVC screw cover.
引文
[1]张居舟,陶固帅,尚光志,等.超高效液相色谱-串联质谱法测定食品塑料包装材料中5种光引发剂及其迁移规律[J].理化检验-化学分册,2017,53(11):1246-1251.
[2]王君,许超,杨学军,等.食品包装用PVC中的物质在5种介质中总迁移规律的研究[J].包装工程,2012,33(19):79-84.
[3]应璐,王全林.以橄榄油为模拟食品测定微波加热容器的总迁移量[J].中国塑料,2009,23(5):99-103.
[4]张佰清,郑贺,邱志隆,等.复合薄膜袋酸性条件下化学物质的总迁移量研究[J].包装工程,2011,32(17):25-28.
[5]王宇,刘坤,张力,等.精炼橄榄油全浸泡法测定食品接触材料的高温总迁移量[J].分析测试学报,2012,31(增刊1):246-250.
[6] SN/T 2818-2011食品接触材料高分子材料橄榄油模拟物中总迁移量的试验方法填充法[S].
[7] SN/T 2334-2009食品接触材料高分子材料橄榄油中总迁移量的试验方法全浸没法[S].
[8] SN/T 2735-2010食品接触材料高分子材料橄榄油模拟物中总迁移量的试验方法袋装法[S].
[9] SN/T 2817-2011食品接触材料高分子材料橄榄油模拟物中总迁移量的试验方法测试池法[S].
[10] SN/T 2824-2011食品接触材料高分子材料总迁移试验条件和方法选择指南[S].
[11] BS EN 1186-1:2002 Materials and articles in contact with foodstuffs-Plastics-Part 1:Guide to the selection of conditions and test methods for overall migration[S].
[12]付善良,丁利,焦艳娜,等.GC-MS/MS用于微波条件下PVC塑料中增塑剂向橄榄油迁移行为的研究[J].分析测试学报,2013,32(5):630-633.
[13] BARNES K A,SINKLAIR C R,WASTON D H.食品接触材料及其化学迁移[M].宋欢,林勤保,主译.北京:中国轻工业出版社,2011:169-170.
[14] GRAUBARDT N,BIEDERMANN M,FISELIER K,et al.Further insights into the mechanism of migration from the PVC gaskets of metal closures into oily foods in glass jars[J].Food Additives&Contaminants:Part A,2009,26(8):1217-1225.
[15]吉玉碧,徐国敏,罗恒,等.软质PVC中增塑剂在不同溶媒中的迁移行为[J].塑料,2012,41(2):41-43.
[16]陈燕芬,钟怀宁,易蓉,等.PVC密封圈中环氧大豆油在食品模拟物中的迁移行为研究[J].现代食品科技,2015,31(8):219-225.
[2]王君,许超,杨学军,等.食品包装用PVC中的物质在5种介质中总迁移规律的研究[J].包装工程,2012,33(19):79-84.
[3]应璐,王全林.以橄榄油为模拟食品测定微波加热容器的总迁移量[J].中国塑料,2009,23(5):99-103.
[4]张佰清,郑贺,邱志隆,等.复合薄膜袋酸性条件下化学物质的总迁移量研究[J].包装工程,2011,32(17):25-28.
[5]王宇,刘坤,张力,等.精炼橄榄油全浸泡法测定食品接触材料的高温总迁移量[J].分析测试学报,2012,31(增刊1):246-250.
[6] SN/T 2818-2011食品接触材料高分子材料橄榄油模拟物中总迁移量的试验方法填充法[S].
[7] SN/T 2334-2009食品接触材料高分子材料橄榄油中总迁移量的试验方法全浸没法[S].
[8] SN/T 2735-2010食品接触材料高分子材料橄榄油模拟物中总迁移量的试验方法袋装法[S].
[9] SN/T 2817-2011食品接触材料高分子材料橄榄油模拟物中总迁移量的试验方法测试池法[S].
[10] SN/T 2824-2011食品接触材料高分子材料总迁移试验条件和方法选择指南[S].
[11] BS EN 1186-1:2002 Materials and articles in contact with foodstuffs-Plastics-Part 1:Guide to the selection of conditions and test methods for overall migration[S].
[12]付善良,丁利,焦艳娜,等.GC-MS/MS用于微波条件下PVC塑料中增塑剂向橄榄油迁移行为的研究[J].分析测试学报,2013,32(5):630-633.
[13] BARNES K A,SINKLAIR C R,WASTON D H.食品接触材料及其化学迁移[M].宋欢,林勤保,主译.北京:中国轻工业出版社,2011:169-170.
[14] GRAUBARDT N,BIEDERMANN M,FISELIER K,et al.Further insights into the mechanism of migration from the PVC gaskets of metal closures into oily foods in glass jars[J].Food Additives&Contaminants:Part A,2009,26(8):1217-1225.
[15]吉玉碧,徐国敏,罗恒,等.软质PVC中增塑剂在不同溶媒中的迁移行为[J].塑料,2012,41(2):41-43.
[16]陈燕芬,钟怀宁,易蓉,等.PVC密封圈中环氧大豆油在食品模拟物中的迁移行为研究[J].现代食品科技,2015,31(8):219-225.
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