Impact of Partitioning in Short-Term Food Contact Applications Focused on Polymers in Support of Migration Modelling and Exposure Risk Assessment

Food contact materials (FCMs) can transfer chemicals arising from their manufacture to food before consumption. Regulatory frameworks ensure consumer safety by prescribing methods for the assessment of FCMs that rely on migration testing either into real-life foods or food simulants. Standard migration testing conditions for single-use FCMs are justifiably conservative, employing recognized worst-case contact times and temperatures. For repeated-use FCMs, the third of three consecutive tests using worst-case conditions is taken as a surrogate of the much shorter contact period that often occurs over the service life of these items. Food contact regulations allow for the use of migration modelling for the chemicals in the FCM and for the partitioning that occurs between the FCM and food/simulant during prolonged contact, under which steady-state conditions are favored. This study demonstrates that the steady-state is rarely reached under repeated-use conditions and that partitioning plays a minor role that results in migration essentially being diffusion controlled. Domains of use have been identified within which partitioning does not play a significant role, allowing modelling based upon diffusion parameters to be used. These findings have the potential to advance the modelling of migration from repeated-use articles for the benefit of regulatory guidance and compliance practices.     

CID-ICP-AES测定碱土金属的分析性能

电荷注入检测器 (CID)配合中阶梯光栅分光系统组成的光谱仪有一些新的特性 ,研究了用CID ICP光谱仪测定碱土金属的分析性能。实验表明 ,碱土 (Be,Mg ,Ca ,Sr,Ba)元素有良好的检出限 :Be ,Sr,Ba 0 0 0 0 2mg·L- 1 ,Mg 0 0 0 0 1mg·L- 1 ,Ca 0 0 0 0 0 3mg·L- 1 ,线性动态范围 10 4 ～ 10 5,自吸收系数均 <1,Ca,Mg的自吸收系数低至 0 7～ 0 8。研究了光度精度与浓度和谱线强度的关系 ,试液浓度在 1mg·L- 1 以上时 ,测定有良好的精密度。     

离子交换固相萃取-气相色谱-质谱联用法测定方便面皮复合包装袋中2,4-二氨基甲苯的迁移量

建立了方便面皮复合包装袋中2,4-二氨基甲苯迁移量的离子交换固相萃取-气相色谱-质谱联用检测方法。样品用4%（v/v）乙酸溶液浸泡,然后采用MCX混合型阳离子交换柱富集净化,以5.0 mL水淋洗小柱,用3.0 mL 5%（v/v）氨化甲醇洗脱样品,洗脱液经过溶剂交换,七氟丁酸酐衍生后,用气相色谱-质谱联用仪对目标物进行检测,外标法定量。2,4-二氨基甲苯在1~50 μg/L范围内,线性相关系数（r）为0.9991,检出限（S/N=3）为0.2 μg/L,定量限（S/N=10）为0.6 μg/L,回收率在89.0%~94.2%之间,相对标准偏差为1.9%~3.6%。该方法的前处理过程无需调节提取液的pH值,也不需要液液萃取,大幅简化了前处理过程,降低了有机溶剂的消耗,具有操作便捷、结果准确的优点,适用于方便面皮复合包装袋中2,4-二氨基甲苯迁移量的检测。     

Comparative study of ink photoinitiators in food packages using gas chromatography with vacuum ultraviolet detection and gas chromatography with mass spectrometry

This work focused on the development and validation of the analytical procedure using gas chromatography equipped with vacuum‐ultraviolet detection for the specific and sensitive determination of nine photoinitiators in food packages. Subsequently, a comparison of the combination of vacuum ultraviolet spectroscopy with gas chromatography and a developed gas chromatography with mass spectrometry method was performed. The vacuum‐ultraviolet spectra of all tested photoinitiators were collected and found to be highly distinct, even for isomers. Under the optimal conditions, the limits of detection for nine photoinitiators ranged from 1 to 5 mg/L using vacuum ultraviolet detection and from 0.15 to 0.5 mg/L using mass spectrometric detection. Both techniques were successfully applied for screening of photoinitiators in seven kinds of food packages and the obtained data showed good agreement (the relative difference was between 3 and 18%). The variability in concentrations found in triplicate samples was assessed to be below 18%. Predominantly benzophenone was found in all analysed samples in the range of 0.31–4.23 mg/kg. It appears to be preferably selected by food packaging manufacturers. This study proposes a new simple and sensitive technique used for analysis of photoinitiators that could be a good alternative to gas chromatography with mass spectrometry.     

基于DMD的区域积分时间可控成像

利用CCD(Charge Coupled Device)相机获取图像后常常存在区域过暗和过曝光的情况,而这两种情况都会掩盖该区域的细节信息。改变CCD相机的积分时间只能对获取的当前帧图像进行单一的积分时间增加或减小,不能同时处理一帧图像中光强过强和过弱的情况。因此针对DMD(Digital Micromirror Device)对每一个微镜片的翻转时间可控的特点,提出了一种区域积分时间可控成像系统,该系统可以通过控制DMD微镜片翻转时间来增加或者减少图像指定区域的积分时间。实验结果表明,该系统可有效地达到同时处理一帧图像中区域过暗和过曝光的目的。     

超声辅助固相萃取分离/ICP-AES测定食品包装铝材中砷的研究

原子光谱法直接测定纯铝材中的砷,受到铝基体的干扰。实验表明,当被测试液中Al的质量浓度大于等于As的5 000倍时,测量误差大于5%。为了降低被测试液中铝的浓度以消除干扰,利用对Al3+吸附作用强的强酸型阳离子交换纤维作为固相萃取剂,通过对萃取剂用量、萃取温度、pH值等条件的研究,得到以下方法：0.900 0 g强酸型阳离子交换纤维在55 ℃,pH 2.0的试液中,对Al3+进行超声辅助萃取5 min,此时以砷酸形式存在的砷不被萃取而留在试液中供测定。结果表明,10.00 mL含砷1.00 μg,铝20.0 mg的试液经过分离后,其中砷未见损失,而残留铝质量浓度约为砷的2 000倍,已不干扰ICP-AES测定As。方法检出限(3 s)为0.027 μg·mL-1,方法定量下限(10 s)为0.091 μg·mL-1。本方法已用于合成样、铝制饮料易拉罐和烘烤食品用铝箔等样品中As的测定,标准加入的回收率98.3%~105%;RSD(n=3) 0.1％~4.3％;结果显示,在本实验所测的铝易拉罐和烘烤用铝箔样品中,砷的含量均低于国家标准(GB/T 3190—2008)的限定值。     

Na2SO4·10H2O基复合相变储能材料对金属封装材料腐蚀性研究

采用失重法,并对腐蚀产物的物质组成和显微结构进行X射线衍射和扫描电镜分析,对十水硫酸钠基复合相变储能材料相变循环对不锈钢、铝合金、纯铜和黄铜等金属封装材料的腐蚀动力学特性进行了研究.结果表明:金属封装材料的耐腐蚀性为不锈钢最佳,紫铜的耐腐蚀性最差,其顺序为:不锈钢304＞不锈钢201＞铝合金1060＞铝合金5052＞铝合金6061＞铝合金7075＞黄铜＞紫铜,纯铜的腐蚀主要以点蚀形式存在,蚀孔表面有Cu2O膜的存在,Cl-的存在与氧竞争吸附,加速腐蚀;黄铜也存在点蚀,同时黄铜与相变材料反应,生成物质粘附在黄铜表面.铝合金腐蚀以点蚀形式存在,腐蚀产物呈开裂状附着于基体表面.铜及合金和铝合金不适合做芒硝基复合相变储能材料的封装材料,不锈钢201和304呈现良好的耐腐蚀状态,适宜作为芒硝基复合相变储能材料的金属封装材料.     

掺铈溴化镧闪烁晶体封装技术的研究

研究了反射层材料、光耦合剂以及晶体表面形态等对φ25.4 mm ×25.4 mm圆柱形晶体样品的闪烁光收集效果的影响,研究结果表明:较有效的光耦合剂为折射率1.54的光学有机硅胶,反射层材料为聚四氟乙烯微粉,闪烁晶体表面形态为入射面粗糙,侧面和出光面抛光.     

超高效液相色谱-串联质谱法测定食品包装材料中全氟辛烷磺酸盐

建立了超高效液相色谱-串联质谱(UPLC- MS/MS)测定食品包装材料中全氟辛烷磺酸盐(PFOS)的方法.采用乙腈作为溶剂,加速溶剂提取法提取食品包装材料中的PFOS.色谱条件:ACQUITY UPLC BEH C₁₈色谱柱（1.7 μm,2.1 mm×50 mm）;柱温:30 ℃;流动相:乙腈/水,梯度洗脱;流速:0.2 mL/min;经UPLC分离后用多级反应监测(MRM)方式测定.用2个子离子的相对丰度定性, 外标法定量.PFOS在0.005～0.500 μg/mL范围内线性良好(R2=0.999),PFOS的回收率为90.0%～101.6%,相对标准偏差RSD为1.5%～3.5%.方法检出限为0.1 μg/m2(S/N≥3).     

LED感应局部加热封装试验研究

采用感应局部加热技术,对大功率发光二极管(LED)封装进行了试验研究。结果表明,由于感应加热对材料和结构具有选择性,封装过程中仅Cu-Sn合金焊料层加热,实现了芯片和覆铜陶瓷基板间的热键合。封装后的LED性能测试表明,该封装技术不仅降低了热阻,使LED在高电流下(4倍电流)仍能保持较低的工作温度,而且降低了热应力和整体高温对芯片结构的损坏,提高了器件性能和可靠性。