Determination of Migration of 1,1'-Sulfonylbis(4-Chlorobenzene) and 4,4'-Dihydroxybiphenyl in Food Contact Material Products by Ultra-High Performance Liquid Chromatography
摘 要
参考GB 5009.156-2016和GB 31604.1-2015,以水、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、95%(体积分数,下同)乙醇溶液、异辛烷等食品模拟物浸泡聚苯砜材质的水杯、奶瓶、螺纹口和涂层罐,前5种食品模拟物的浸泡液直接过0.22 μm滤膜,滤液采用超高效液相色谱法(UHPLC)分析。分取95%乙醇溶液和异辛烷浸泡液各10 mL,于50℃,5 000 Pa条件下旋转蒸发至近干,用70%(体积分数)甲醇溶液溶解、定容至10 mL,过0.22 μm滤膜,滤液采用UHPLC分析。以ACQUITY UPLC BEH C18色谱柱作固定相,以不同体积比甲醇和水的混合溶液作流动相进行梯度洗脱,在检测波长247 nm下进行检测。结果显示,7种食品模拟物中的两种目标物可在6.500 min以内实现完全分离,其中1,1'-磺酰基二(4-氯苯)和4,4'-联苯二酚的质量浓度分别在0.03~0.40 mg·L-1和0.3~4.0 mg·L-1内与峰面积呈线性关系,测定下限(10S/N)分别为0.015~0.030 mg·kg-1和0.023~0.030 mg·kg-1;3个浓度水平下的加标回收率为89.0%~110%,测定值的相对标准偏差(n=6)为1.9%~6.7%;方法用于10批实际样品的分析,两种目标物的测定值均小于测定下限,符合GB 4806.6-2016和GB 9685-2016的特定迁移限量要求。
Abstract
Referring to GB 5009.156-2016 and GB 31604.1-2015, food simulants including water, 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50% (volume fraction) ethanol solution, 95% (volume fraction, the same below) ethanol solution and isooctane were used to immerse water cups, milk bottles, threaded ports and coating cans with polystyrene sulfone material. The soak solution of the first 5 food simulants was directly passed through a 0.22 μm filter membrane, and the filtrate was analyzed by ultra-high performance liquid chromatography (UHPLC). An aliquot (10 mL) of 95% ethanol solution or isooctane soak solution was taken, and evaporated to near dryness by rotating at 50℃ and 5 000 Pa. The residue was dissolved and diluted to 10 mL by 70% (volume fraction) methanol solution, and the solution obtained was passed through a 0.22 μm filter membrane. The filtrate was analyzed using UHPLC. The ACQUITY UPLC BEH C18 chromatographic column was used as the stationary phase, and mixed solutions composed of methanol and water at different volume ratios were used as the mobile phase for gradient elution. The detection was performed at a detection wavelength of 247 nm. It was shown that the 2 targets in the 7 food simulants could be completely separated within 6.500 min, and linear relationships between values of the mass concentration of 1,1'-sulfonylbis(4-chlorobenzene) and 4,4'-dihydroxybiphenyl and the peak area were kept in the ranges of 0.03-0.40 mg·L-1 and 0.3-4.0 mg·L-1, with lower limits of determination (10S/N) in the range of 0.015-0.030 mg·kg-1 and 0.023-0.030 mg·kg-1, respectively. Test for recovery was made at the 3 concentration levels by standard addition method, giving recoveries in the range of 89.0%-110%, and RSDs (n=6) of the determined values ranged from 1.9% to 6.7%. The proposed method was applied to the analysis of 10 batches of actual samples, and the determined values of the 2 targets were lower than the lower limits of determination, meeting the requirements of specific migration limits of GB 4806.6-2016 and GB 9685-2016.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202308007
所属栏目 工作简报
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收稿日期 2021/12/15
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备注望秀丽,高级工程师,博士,主要从事轻纺消费品中有毒有害物质的检测,wangxiuli19840603@163.com
引用该论文: WANG Xiuli,QUAN Wangsun,GUAN Li. Determination of Migration of 1,1'-Sulfonylbis(4-Chlorobenzene) and 4,4'-Dihydroxybiphenyl in Food Contact Material Products by Ultra-High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(8): 911~916
望秀丽,全王榫,管理. 超高效液相色谱法测定食品接触材料制品中1,1'-磺酰基二(4-氯苯)和4,4'-联苯二酚的迁移量[J]. 理化检验-化学分册, 2023, 59(8): 911~916
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参考文献
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【2】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:GB 9685-2016[S].北京:中国标准出版社, 2017.
【3】周韵,清江,马明,等.气相色谱-三重串联四极杆质谱法测定聚醚砜水杯中4,4'-二氯二苯砜迁移量[J].环境化学, 2014,33(10):1808-1810.
【4】李宁,王丹,张小明,等.HPLC测定塑料食品接触材料中4,4'-联苯二酚和4,4'-二氯二苯砜迁移量[J].现代食品, 2020(17):174-178.
【5】赵镭,李文慧,李洁君,等.HPLC法测定4,4'-联苯二酚和4,4'-二氯二苯砜迁移量[J].食品工业, 2021,42(4):471-474.
【6】王涛,马明,邵敏,等.高效液相色谱法同时测定塑料食品接触材料中双酚S、双酚A和4,4'-二氯二苯砜的迁移量[J].理化检验-化学分册, 2017,53(12):1398-1402.
【7】谢文缄,席绍峰,谢永萍,等.高效液相色谱法测定食品模拟物中的二羟基联苯和二氯二苯砜[J].理化检验-化学分册, 2016,52(9):1100-1103.
【8】康峰,赵金尧,刘钊,等.超高效液相色谱法测定食品接触材料中间苯二甲酸和对苯二甲酸特定迁移量[J].理化检验-化学分册, 2021,57(5):398-404.
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