顶空-气相色谱法测定聚丙烯腈类食品接触材料中3种腈类化合物残留量
|
摘要
建立了顶空-气相色谱法测定聚丙烯腈类食品接触材料中3种腈类化合物残留量的分析方法。通过优化前处理溶剂种类、溶剂体积、样品前处理溶解时间,以及平衡温度和时间等色谱条件,实现了对3种腈类化合物残留量的常规、快速分析。结果表明:3种腈类化合物在完全分离的前处理和色谱条件下,在0.02～2.0 mg/L质量浓度范围内线性关系良好,线性相关系数均大于0.999;3种腈类化合物的方法定量限(10S/N)为0.045～0.052 mg/kg,低、中、高质量分数的回收率为89.4%～110.7%,相对标准偏差(RSD)为3.5%～9.8%;方法满足了聚丙烯腈类食品接触产品中3种腈类化合物残留量的检测要求。实际检测中发现丙烯腈-丁二烯-苯乙烯共聚物(ABS)和丙烯腈-苯乙烯共聚物(AS)材质除含有较高的丙烯腈外,还含有一定量的丙腈和乙腈单体,因此需要关注AS和ABS材质等食品接触材料产品中存在腈类化合物的风险。
A headspace-gas chromatography method was developed for the determination of residual amounts of three nitrile compounds in polyacrylonitrile food contact materials. By optimizing the pretreatment conditions such as the type of solvent, the volume of solvent, the dissolution time of the sample, and the chromatographic conditions such as equilibrium temperature and time, the conventional and rapid analysis of the residual amount of three nitrile compounds was realized.The results showed that the three nitrile compounds could be separated completely under the pretreatment and chromatographic conditions, the linear relationship was good in the concentration range of 0.02-2.0 mg/L, and the linear correlation coefficient was greater than 0.999. The detection limit with 10 S/N was 0.045-0.052 mg/kg, the recovery rate of low, medium and high content was 89.4%-110.7%, and the relative standard deviation(RSD) was 3.5%-9.8%. The detection requirements of residual amounts of three nitrile compounds in the food contact products of polyacrylonitrile were satisfied. In the actual test, it was found that acrylonitrile-butadiene-styrene(ABS) and acrylonitrile-styrene(AS) materials not only contained more acrylonitrile, but also contained certain acrylonitrile and acetonitrile monomers. Therefore, it is necessary to pay attention to the risk of nitrile compounds in food contact materials such as AS and ABS.
A headspace-gas chromatography method was developed for the determination of residual amounts of three nitrile compounds in polyacrylonitrile food contact materials. By optimizing the pretreatment conditions such as the type of solvent, the volume of solvent, the dissolution time of the sample, and the chromatographic conditions such as equilibrium temperature and time, the conventional and rapid analysis of the residual amount of three nitrile compounds was realized.The results showed that the three nitrile compounds could be separated completely under the pretreatment and chromatographic conditions, the linear relationship was good in the concentration range of 0.02-2.0 mg/L, and the linear correlation coefficient was greater than 0.999. The detection limit with 10 S/N was 0.045-0.052 mg/kg, the recovery rate of low, medium and high content was 89.4%-110.7%, and the relative standard deviation(RSD) was 3.5%-9.8%. The detection requirements of residual amounts of three nitrile compounds in the food contact products of polyacrylonitrile were satisfied. In the actual test, it was found that acrylonitrile-butadiene-styrene(ABS) and acrylonitrile-styrene(AS) materials not only contained more acrylonitrile, but also contained certain acrylonitrile and acetonitrile monomers. Therefore, it is necessary to pay attention to the risk of nitrile compounds in food contact materials such as AS and ABS.
引文
[1]周洪柱,崔云彪,李光.毛细管气相色谱法测定丙烯腈中微量杂质[J].应用化工,2009,28(4):617-619.
[2]向彩红,叶英,范军,等.顶空-气相色谱法测定土壤和沉积物中丙烯醛、丙烯腈、乙腈含量[J].环境化学,2017,36(2):456-458.
[3]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品接触材料及制品用添加剂使用标准:GB9685-2016[S].北京:中国标准出版社,2017.
[4]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品接触用塑料树脂:GB 4806.6-2016[S].北京:中国标准出版社,2017.
[5]中华人民共和国国家卫生和计划生育委员会.生活饮用水卫生标准:GB5749-2006[S].北京:中国标准出版社,2007.
[6]On plastic materials and article s intended to come into contact with food:Commission Regulation(EU)No 10/2011[S].
[7]马明,沈康俊,邵敏.顶空-气相色谱-质谱法测定食品接触ABS,AS制品中丙烯腈[J].分析试验室,2017,36(6):685-689.
[8]谢永萍.顶空-气相色谱-质谱法测定丙烯腈-丁二烯-苯乙烯玩具中丙烯腈单体的含量[J].理化检验:化学分册,2015,51(9):1282-1285.
[9]朱文亮,周勇,陈晓鹏,等.顶空气相色谱法测定丙烯腈-苯乙烯(AS)塑料中残留的7种单体[J].食品工业科技,2012,33(13):322-324,382.
[10]邵秋荣,丁晓,邵劲勤,等.GC-MS法测定ABS,SAN中残留苯乙烯和丙烯腈单体[J].化学分析计量,2015,24(1):80-82.
[11]李丽.丙烯腈-丁二烯-苯乙烯塑料残留单体含量的研究[J].炼油与化工,2016,27(6):62-63.
[12]黄丹,陈莉,颜林平,等.顶空气相色谱法测定食品级AS和ABS色母粒中丙烯腈残留量[J].塑料科技,2016,44(4):86-89.
[13]张月华.丙烯腈单体测定的方法比较研究[J].食品安全导刊,2015(12):103-105.
[14]赵亚婷,张颖,李思睿,等.气相色谱法测定丁二烯尾气中乙腈和N,N-二甲基甲酰胺的含量[J].石油化工,2016,45(3):352-354.
[15]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品接触材料及制品丙烯腈的测定和迁移量的测定:GB 31604.17-2016[S].北京:中国标准出版社,2017.
[16]苏莉.气相色谱法测定聚和物多元醇微量丙烯腈和苯乙烯含量[J].天津化工,2017,31(5):42-43.
[17]袁丽凤,邬蓓蕾,崔家玲,等.丙烯腈-丁二烯-苯乙烯(ABS)塑料中残留单体的溶解沉淀-气相色谱法测定[J].分析测试学报,2008,27(10):1095-1098.
[2]向彩红,叶英,范军,等.顶空-气相色谱法测定土壤和沉积物中丙烯醛、丙烯腈、乙腈含量[J].环境化学,2017,36(2):456-458.
[3]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品接触材料及制品用添加剂使用标准:GB9685-2016[S].北京:中国标准出版社,2017.
[4]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品接触用塑料树脂:GB 4806.6-2016[S].北京:中国标准出版社,2017.
[5]中华人民共和国国家卫生和计划生育委员会.生活饮用水卫生标准:GB5749-2006[S].北京:中国标准出版社,2007.
[6]On plastic materials and article s intended to come into contact with food:Commission Regulation(EU)No 10/2011[S].
[7]马明,沈康俊,邵敏.顶空-气相色谱-质谱法测定食品接触ABS,AS制品中丙烯腈[J].分析试验室,2017,36(6):685-689.
[8]谢永萍.顶空-气相色谱-质谱法测定丙烯腈-丁二烯-苯乙烯玩具中丙烯腈单体的含量[J].理化检验:化学分册,2015,51(9):1282-1285.
[9]朱文亮,周勇,陈晓鹏,等.顶空气相色谱法测定丙烯腈-苯乙烯(AS)塑料中残留的7种单体[J].食品工业科技,2012,33(13):322-324,382.
[10]邵秋荣,丁晓,邵劲勤,等.GC-MS法测定ABS,SAN中残留苯乙烯和丙烯腈单体[J].化学分析计量,2015,24(1):80-82.
[11]李丽.丙烯腈-丁二烯-苯乙烯塑料残留单体含量的研究[J].炼油与化工,2016,27(6):62-63.
[12]黄丹,陈莉,颜林平,等.顶空气相色谱法测定食品级AS和ABS色母粒中丙烯腈残留量[J].塑料科技,2016,44(4):86-89.
[13]张月华.丙烯腈单体测定的方法比较研究[J].食品安全导刊,2015(12):103-105.
[14]赵亚婷,张颖,李思睿,等.气相色谱法测定丁二烯尾气中乙腈和N,N-二甲基甲酰胺的含量[J].石油化工,2016,45(3):352-354.
[15]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品接触材料及制品丙烯腈的测定和迁移量的测定:GB 31604.17-2016[S].北京:中国标准出版社,2017.
[16]苏莉.气相色谱法测定聚和物多元醇微量丙烯腈和苯乙烯含量[J].天津化工,2017,31(5):42-43.
[17]袁丽凤,邬蓓蕾,崔家玲,等.丙烯腈-丁二烯-苯乙烯(ABS)塑料中残留单体的溶解沉淀-气相色谱法测定[J].分析测试学报,2008,27(10):1095-1098.