食品接触用硅橡胶中8种金属元素的迁移分析

目的 研究食品接触用硅橡胶制品中8种金属元素(钡、锂、铜、铁、钴、锰、锌和铝)的迁移量。方法 以3%乙酸(m:V)作为食品模拟物, 利用电感耦合等离子体质谱法测定食品接触用硅橡胶中8种金属元素的迁移量。结果 各金属元素的线性范围在1~100 μg/L, 方法检出限在0.005~0.6 μg/kg之间, 加标回收率在88.4%~108.0%, 重复性测定相对偏差(n=6)在1.2%~3.6%之间。对20批次食品接触用硅橡胶制品中8种金属元素的迁移量进行测试, 发现7种金属元素(钡、锂、铜、铁、锰、锌和铝)均有检出。结论 该方法可以准确测定食品接触用硅橡胶中8种金属元素(钡、锂、铜、铁、钴、锰、锌和铝)的迁移量, 且检测结果显示随着迁移次数的增加迁移量逐渐降低。     

食品接触橡胶制品中N-亚硝胺迁移量的 风险分析

建立气相色谱-质谱联用测定食品接触橡胶制品中13种N-亚硝胺迁移量的方法,并调查餐具器皿产品中N-亚硝胺的迁移水平。样品经50%乙醇浸提、固相萃取柱富集净化、氮吹浓缩后上机测试,外标法定量。在本试验条件下,13种N-亚硝胺线性关系良好,检出限符合要求,回收率为79.3%～91.4%,RSD为1.73%～3.22%,该方法简便快捷,结果准确可靠。采用该方法对网购的样品进行分析测试发现,有5批次样品检出N-亚硝胺,迁移水平在0.014～0.074 mg/kg之间,检出率为25%,表明该类产品中存在N-亚硝胺迁移风险。     

电感耦合等离子体质谱法检测食品接触用铝箔在不同迁移条件下的铝迁移量

目的系统研究食品接触用铝箔纸中铝的迁移条件和检测方法。方法结合食品接触用铝箔纸实际接触条件,模拟3种迁移实验条件,采用电感耦合等离子体质谱法进行对铝迁移量检测。结果该方法检出限为0.5μg/L,线性范围宽,加标回收率为87.0%～99.2%,相对标准偏差(relative standard deviation,RSD)在0.4%～5.5%(n=6)。结论建立的方法适合食品接触用材料铝箔在不同迁移条件下的铝迁移量的检测。     

电感耦合等离子体发射光谱法测定食品接触用无机材料及制品中13种重金属迁移量

目的 建立一种同时检测食品接触用无机材料及制品中13种重金属迁移量(铝、砷、钡、镉、钴、铬、铜、锰、镍、铅、锑、硒与锌)的电感耦合等离子体发射光谱(inductively coupled plasma atomic emission spectrometry, ICP-AES)法。方法 采用4%(V:V)醋酸溶液, 在特定迁移实验条件下, 避光浸泡试样, 优化仪器参数和实验条件, 用电感耦合等离子体发射光谱法同时测定浸泡液中13种元素迁移量。结果 该方法检出限为0.001~0.010 mg/L, 样品的加标回收率为90.8%~105.1%, 相对标准偏差为0.96%~3.89%。结论 该方法简便、快速、高效、灵敏度高, 为食品接触用无机材料及制品中多种痕量有害元素迁移量进行合理产品风险评估提供一种高效、可行的手段。     

电感耦合等离子体发射光谱法测定食品接触用搪瓷制品中11种重金属迁移量

目的 建立电感耦合等离子体发射光谱法(inductively coupled plasma atomic emission spectroscopy, ICP-AES)同时检测食品接触用搪瓷制品中11种重金属(铝、砷、钡、镉、钴、铬、锰、镍、铅、锑、锌)迁移量的分析方法。方法 采用4%(V:V)乙酸溶液, 在特定迁移试验条件下, 避光浸泡试样, 优化仪器参数和实验条件, 用电感耦合等离子体发射光谱法同时测定浸泡液中11元素迁移量。结果 方法检出限为0.001~0.010 mg/L, 样品加标回收率为92.2%~105.5%, 相对标准偏差为0.91%~3.65%。结论 方法操作简便, 准确度好, 灵敏度高、检出限低, 为食品接触用搪瓷制品中多种痕量有害元素迁移量进行合理产品风险评估提供一种高效、可行的手段。针对国标GB 4806.3-2016《食品安全国家标准搪瓷制品》中理化指标与迁移试验提出合理建议。     

食品接触材料油脂模拟物中总迁移量的探讨

总迁移量作为食品接触材料的关键的卫生性能指标之一,是企业质量控制和政府监督管理中的重要参数。油脂模拟物中总迁移量反映了预期接触油脂类食品接触材料的质量安全。实验室目前多采用有机溶剂替代橄榄油进行测试,但是替代试验结果往往存在偏差,难以反应正确真实的迁移情况。本文比较了国内外油脂类总迁移量的检测方法,探究了橄榄油与有机溶剂总迁移量差异,为改进我国总迁移量检测方法提供一些依据和参考。     

LC-MS法测定食品接触用PET材料食品模拟物中间苯二甲酸和对苯二甲酸的迁移量

目的：建立食品接触用PET材料食品模拟物中间苯二甲酸和对苯二甲酸迁移量的高效液相色谱-串联质谱的检测方法。方法：样品经食品模拟物浸泡后,对食品模拟物进行检测,采用负离子扫描(ESI^-)和多反应检测(MRM)模式进行检测,外标法进行定量分析。结果：各种模拟物中间苯二甲酸和对苯二甲酸分离度良好,在50～1 000 ng·mL^-1线性良好(r²均达到0.998以上),水基、酸性食品、酒精类和油基食品模拟物检出限为10 ng·mL^-1,定量限为30 ng·mL^-1,回收率极小值为93.6%、极大值为103.9%,RSD最大值为1.34%(n=6)。结论：该方法简单、准确可靠,能快速检测出目标物质,填补了国家标准中间苯二甲酸检测方法缺失的空白,还能同时实现间苯二甲酸和对苯二甲酸的定量检测,可大大缩短检测时间。     

食品用塑料包装中壬基酚迁移量的检测

建立高效液相色谱-串联质谱法测定食品用塑料包装中壬基酚的迁移量。样品经迁移试验得食品模拟物,水性模拟物直接上机,油基模拟物经甲醇提取、冷冻离心后取上清液分析,外标法定量。在本试验条件下,壬基酚线性关系良好,6种模拟物的相关系数都达到0.998 5以上,两类模拟物的检出限分别为0.01 mg/L和0.01 mg/kg,回收率为89.3%～94.4%,RSD值为2.76%～3.37%。该法简单、灵敏、准确,适用于食品用塑料包装中壬基酚迁移量的检测。     

电感耦合等离子体质谱法同时测定食品接触用金属制品中16种金属元素的迁移量

目的 对食品接触用金属制品中16种金属元素在酸性条件(4%乙酸溶液)下迁移检测方法进行系统的研究。方法 结合食品接触用金属制品实际接触条件,选择4%乙酸溶液煮沸30min,重复三次前处理条件,两种适合的内标元素,采用了电感耦合等离子体质谱法同时测定16种元素进行检测。结果 该方法汞镉元素定量检出限为0.1μg /L,其余元素为0.5μg /L,线性范围宽,加标回收率结果令人满意,RSD在0.3%~7.4%(n=6),适合食品接触用金属制品中16种金属元素迁移量的检测。结论 通过比较检测数据,铝合金、铁制品中的砷、铝、铁元素迁移量较高,存在产品合格不安全的质量安全隐患,应该引起食品相关产品监督部门的高度重视！     

食品接触用硅橡胶中3种环硅氧烷的测定及迁移规律

采用溶剂提取-气相质谱联用法(Solvent extraction-gas chromatography/mass spectrometry,solvent extraction-GC/MS)测定食品接触用硅橡胶中八甲基环四硅氧烷(Octamethylcyclotetrasiloxane,D4)、十甲基环五硅氧烷(Decamethylcyclopentasiloxane,D5)和十二甲基环六硅氧烷(Dodecamethylcyclohexasiloxane,D6)等3种环硅氧烷的含量,并研究硅橡胶烤盘中D4~D6向油性食品模拟物中的迁移规律。采用衰减全反射-傅里叶变换红外光谱(Attenuated total reflectance-Fourier transform infrared spectroscopy,ATR-FTIR)分析方法确定硅橡胶的材质,以优化的提取溶剂正己烷和超声提取时间30 min,通过GC/MS检测3种不同用途的9个硅橡胶品牌产品中D4~D6的含量。以其中一种硅橡胶烤盘进行单面迁移试验。结果表明:D4~D6在0.5~20.0 μg/mL质量浓度范围内线性良好,决定系数R²大于0.9961,且D4~D6的检出限均小于为11.2 ng/mL,定量限均小于37.2 ng/mL。通过加标验证,D4~D6的平均回收率为85.20%~98.12%,相对偏差RSD为2.17%~4.27%(n=6)。硅橡胶奶嘴和高压锅密封圈中D4~D6含量较少,而硅橡胶烤盘中含量最多,其D4~D6的均值分别为175.08、824.12和901.17 mg/kg。通过迁移试验,发现硅橡胶烤盘在60 ℃油性食品模拟物95%乙醇中达到迁移平衡时,D4~D6的迁移率分别为71.36%、57.03%和49.31%。这表明D4~D6会迁移到油性食品中,且分子量较小的D4更易迁出,其安全性不可忽视。     

Progress in research on the safety of silicone rubber products in food processing

Silicone rubber (SR) is widely used in the food processing industry due to its excellent physical and chemical properties. However, due to the differences in SR product production formulas and processes, the quality of commercially available SR products varies greatly, with chemical and biological hazard potentials. Residual chemicals in SR, such as siloxane oligomers and 2,4-dichlorobenzoic acid, are non-intentionally added substances, which may migrate into food during processing so the safe use of SR must be guaranteed. Simultaneously, SR in contact with food is susceptible to pathogenic bacteria growing and biofilm formation, like Cronobacter sakazakii, Staphylococcus aureus, Salmonella enteritidis, and Listeria monocytogenes, posing a food safety risk. Under severe usage scenarios such as high-temperature, high-pressure, microwave, and freezing environments with long-term use, SR products are more prone to aging, and their degradation products may pose potential food safety hazards. Based on the goal of ensuring food quality and safety to the greatest extent possible, this review suggests that enterprises need to prepare high-quality food-contact SR products by optimizing the manufacturing formula and production process, and developing products with antibacterial and antiaging properties. The government departments should establish quality standards for food-contact SR products and conduct effective supervision. Besides, the reusable SR products should be cleaned by consumers immediately after use, and the deteriorated products should be replaced as soon as possible.     

高效液相色谱法检测食品接触用硅橡胶制品中2,4-二氯苯甲酸的迁移量

目的 建立6种食品模拟物中2,4-二氯苯甲酸的定量检测方法,并对食品接触用硅橡胶制品中2,4-二氯苯甲酸迁移行为进行研究.方法 各食品模拟物中2,4-二氯苯甲酸采用Aq-C18色谱柱进行分离,以乙腈和0.025％磷酸水溶液作为流动相,高效液相色谱法(high performance liquid chromatogra...     

Determination of siloxanes in silicone products and potential migration to milk,formula and liquid simulants

A pressurised solvent extraction procedure coupled with a gas chromatography–mass spectrometry–selective ion monitoring (GC–MS–SIM) method was developed to determine three cyclic siloxanes, octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6) and three linear siloxanes, octamethyltrisiloxane (L3), decamethyltetrasiloxane (L4), dodecamethylpentasiloxane (L5), in silicone products. Additionally, two different extraction methods were developed to measure these siloxanes migrating into milk, infant formula and liquid simulants (50 and 95% ethanol in water). The limits of quantification (LOQs) of the six siloxanes ranged from 6?ng/g (L3) to 15?ng/g (D6). Silicone nipples and silicone bakewares were extracted using pressurised solvent extraction (PSE) and analysed using the GC–MS–SIM method. No linear siloxanes were detected in the silicone nipple samples analysed. The three cyclic siloxanes (D4, D5 and D6) were detected in all silicone nipple samples with concentrations ranging from 0.5 to 269?µg/g. In the bakeware samples, except for L3, the other five siloxanes were detected with concentrations ranging from 0.2?µg/g (L4) to 7030?µg/g (D6). To investigate the potential migration of the six siloxanes from silicone nipples to milk and infant formula, a liquid extraction and dispersive clean-up procedure was developed for the two matrices. The procedure used a mix of hexane and ethyl acetate (1?:?1, v/v) as extraction solvent and C₁₈ powder as the dispersive clean-up sorbent. For the liquid simulants, extraction of the siloxanes was achieved using hexane without any salting out or clean-up procedures. The recoveries of the six siloxanes from the milk, infant formula and simulants fortified at 50, 100, 200, 500 and 1000?µg/l ranged from 70 to 120% with a relative standard derivation (RSD) of less than 15% (n?=?4). Migration tests were performed by exposing milk, infant formula and the liquid simulants to silicone baking sheets with known concentrations of the six siloxanes at 40°C. No siloxanes were detected in milk or infant formula after 6?h of direct contact with the silicone baking sheet plaques, indicating insignificant migration of the siloxanes to milk or infant formula. Migration tests in the two simulants lasted up to 72?h and the three cyclic siloxanes were detected in 50% ethanol after an 8-h exposure and after 2?h in 95% ethanol. The highest detected concentrations of D4, D5 and D6 were 42, 36 and 155?ng/ml, respectively, indicating very limited migration of D4, D5 or D6 into the two simulants.     

HPLC法同时测定食品接触橡胶密封垫圈中3种醛类化合物迁移量

目的:建立一种利用HPLC同时测定食品接触橡胶密封垫圈中甲醛、乙醛和丙烯醛迁移量的分析方法。方法:以4%乙酸水溶液、10%乙醇水溶液、20%乙醇水溶液、50%乙醇水溶液及橄榄油作为食品模拟物,按GB 5009.156—2016进行迁移试验,经衍生化反应后,采用Accucore RP-MS色谱柱分离,以乙腈—水溶液为流动相等度洗脱,紫外检测器检测。结果:3种醛类化合物在0.05~5.00 mg/L内呈良好的线性关系,相关系数R²≥0.9983。甲醛、乙醛和丙烯醛检出限分别为0.58,0.62,1.68 mg/kg;定量限分别为0.98,0.99,2.93 mg/kg,在1.0~15.0 mg/kg添加水平范围内,3种醛类化合物回收率为81.0%~103.3%;相对标准偏差为0.78%~7.05%。结论:该方法适用于食品接触橡胶密封垫圈中醛类化合物迁移量的检测。     

反相高效液相色谱法测定婴幼儿配方食品中的叶黄素

建立了反相高效液相色谱法测定婴幼儿配方食品中叶黄素测定方法。选用色谱柱YMC Carotenoid4.6mm×250mm,5μm,以甲醇、甲基叔丁基醚为流动相进行梯度洗脱,流速为1mL/min,于445nm波长下,测定婴幼儿配方食品中叶黄素的含量,叶黄素含量在0.0164～0.492μg/mL范围内呈线性关系,R=0.9998,平均回收率为99.2%,RSD为1.1%。该方法可以简便准确的测定婴幼儿配方食品中叶黄素的含量。     

上海市流通市场中烘焙用硅橡胶制品中挥发性物质含量的调查

目的 调查上海市烘焙用硅橡胶制品中的挥发性物质的含量。方法 参照GB 28482-2012《婴幼儿安抚奶嘴安全要求》的检测方法。结果 在30批次烘焙用硅橡胶制品, 仅有5批次样品的挥发性物质含量小于参考值, 83.3%的样品中的挥发性物质的含量都大于0.5%, 且80%的挥发性物质含量都超出参考值的3~5倍。结论 通过对30批次烘焙用硅橡胶制品中挥发性物质的检测, 发现这类产品中挥发性物质含量过高。     

食品接触材料用硅橡胶检测研究进展

硅橡胶以其优良的稳定性和安全性被广泛应用于食品接触材料领域,随着硅橡胶在食品工业上的广泛应用,其使用过程中的安全性也逐渐受到人们的重视。本文综述了食品接触材料用硅橡胶中可能迁移出的有毒物质,列举了国际上关于食品接触用硅橡胶材料的相关检测标准及法规,介绍了分析推断硅橡胶老化机制的仪器分析方法,总结了食品接触用硅橡胶制品迁移到食品或食品模拟液中的环硅氧烷和重金属离子等有毒物质的具体检测方法。目前,在日常食品接触用硅胶制品的使用过程中,迁移到食品中最多的有害物质是挥发性环硅氧烷,国内外主要应用气相色谱法、气质联用法或核磁共振法来定性定量分析检测迁移到食品中的环硅氧烷。本文旨在对日常使用过程中硅橡胶的安全性的判断及国内食品接触用硅橡胶材料标准的制定提供一定的参考。     

Potential silver nanoparticles migration from commercially available polymeric baby products into food simulants

In recent years, silver nanoparticles (AgNPs) have been extensively employed in food packaging systems as a potential antibacterial agent. Although proven to be highly effective, the increased number of AgNP-containing products raises concerns among consumers regarding the migration of AgNPs from the packaging material into foods, which may exert toxic effects. To address this, five baby products were chosen (baby bottle A, baby bottle B, pacifier A, pacifier B and breastmilk storage bag) to investigate AgNPs migration into three food simulants (deionised water, 4% acetic acid (w/v) and 50% ethanol (v/v)) using inductively coupled plasma mass spectrometry (ICP-MS). As a result, the highest level of migrated Ag was observed for 4% acetic acid in the case of baby bottle B, pacifier A, pacifier B and the breastmilk storage bag, with the detection amount ranging from 1.05–2.25 ng/mL. On the other hand, baby bottle A showed the maximum migration for 50% ethanol due to the polymer nature. Finally, a centrifugal ultrafiltration experiment was conducted to determine the fraction of dissolved Ag in acidic simulant and it was found that migrated Ag was predominantly in Ag⁺ form, with a small fraction of non-ionic AgNPs. Thus, it has been found that the amount of migrated Ag in baby products was low; however, the migration was dependent on the type of food simulant and polymer nature.