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

望秀丽; 全王榫; 管理

doi:10.11973/lhjy-hx202308007

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

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

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.

HTML全文

参考文献(9)

施引文献

资源附件(0)