摘要
建立了超高效液相色谱法(UHPLC)测定食品接触材料聚对苯二甲酸乙二醇酯(PET)中的间苯二甲酸和对苯二甲酸特定迁移量的方法。按照以下参数进行迁移试验:①参考方法为国家标准GB 5009.156-2016和GB/T 23296.1-2009;②模拟液为4%(体积分数)乙酸溶液、10%(体积分数)乙醇溶液、20%(体积分数)乙醇溶液、50%(体积分数)乙醇溶液和橄榄油;③迁移温度为70℃,迁移时间为2h。得到的迁移溶液供UHPLC进行分析,选择ShimSen-VD C 30色谱柱为固定相,以体积比为40∶60的甲醇和7.5mmol·L^(-1)磷酸二氢钾-磷酸缓冲溶液(pH 3.0)的混合溶液为流动相进行等度洗脱,在230nm处用二极管阵列检测器(DAD)测定。以邻苯二甲酸为内标、用5种模拟液配制混合标准溶液系列,结果表明:对苯二甲酸、间苯二甲酸的线性范围为0.5~15.0mg·L^(-1),检出限(3S/N)为0.03~0.07mg·L^(-1)。对实际样品进行3个浓度水平的加标回收试验,得到对苯二甲酸、间苯二甲酸的回收率为92.4%~106%,测定值的相对标准偏差(n=6)为0.17%~5.0%。用此方法分析了PET样品,未发现有这两种物质的迁移。
A method was developed for the simultaneous determination of migration amount of m-phthalic acid and p-phthalic acid in food contact material of ethylene terephthalate(P ET)by ultra high performance liquid chromatography(U HPLC).Parameters for migration test were as follows:①national standards of GB 5009.156-2016and GB/T 23296.1-2009were adopted as reference methods;②4%(volume fraction)acetic acid solution,10%(volume fraction)ethanol solution,20%(volume fraction)ethanol solution,50%(volume fraction)e thanol solution and olive oil were used as simulant solutions;③migration temperature was 70℃,and migration time was 2h.The obtained migration solution was analyzed by UHPLC.ShimSen-VD C30 chromatographic column was selected as the stationary phase.The mixture of methanol and 7.5 mmol·L^(-1) potassium dihydrogen phosphate-phosphate buffer solution(pH 3.0)at volume ratio of 40∶60was used as the mobile phase for isocratic elution,a nd the content of p-phthalic acid and m-phthalic acid was determined with DAD at 230nm.Using phthalate as the internal standard,a series of mixed standard solutions were prepared with above 5simulant solutions.The results showed that linearity ranges of p-phthalic acid and m-phthalic acid was found within 0.5-15.0 mg·L^(-1),w ith detection limits(3 S/N)in the range of 0.03-0.07 mg·L^(-1).The spiked recovery test was made on the actual sample at three concentration levels,giving results of p-phthalic acid and m-phthalic acid in the range of 92.4%-106%,and RSDs(n=6)of the determined values(n=6)ranged from 0.17%to 5.0%.The PET samples were analyzed by the proposed method,and no migration of these two substances was found.
作者
康峰
赵金尧
刘钊
周丛
万富
谭宇诗
王莉
KANG Feng;ZHAO Jinyao;LIU Zhao;ZHOU Cong;WAN Fu;TAN Yushi;WANG Li(Hu′nan Testing Institute of Product and Commodity Supervision,Changsha 410007,China;College of Resources&Environment,Hu′nan Agricultural University,Changsha 410128,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2021年第5期398-404,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
湖南省质检院科研项目(2018TD18-02)
湖南省市场监督管理局科研项目(2021KJJH39)。
关键词
超高效液相色谱法
间苯二甲酸
邻苯二甲酸
迁移量
食品接触材料
ultra high performance liquid chromatography
m-phthalic acid
p-phthalic acid
migration
f ood contact material
