不同结构聚丙烯中紫外线吸收剂的迁移

目的探究温度、时间、食品模拟物、材料结构及添加剂分子等对聚丙烯中3种紫外线吸收剂迁移的影响。方法建立3种紫外线吸收剂(UV-P,UV-531,UV-327)的高效液相色谱检测方法。再在20,40,70°C下,研究添加剂向5种食品模拟物的迁移。结果添加剂在0.1~20μg/m L内线性良好(R0.99),检出限为0.03~0.05μg/m L。加标含量为每克塑料中添加20,80,200μg紫外线吸收剂时,回收率为81.6%~99.8%,相对标准偏差为2.3%~7.7%。在体积分数为10%的乙醇和质量分数为3%的乙酸溶液中,未检出添加剂;在体积分数为20%的乙醇溶液中,只检测到UV-P;在体积分数为50%的乙醇溶液和异辛烷中,3种紫外线吸收剂均被检测到。结论升高温度、延长时间,紫外线吸收剂迁移量逐渐增加直到平衡;紫外线吸收剂易于向异辛烷和乙醇溶液迁移,乙醇溶液中,随着乙醇含量的增加,发生迁移的添加剂种类和质量也随之增加;紫外线吸收剂的迁移量随着聚丙烯材料结晶度的增加而减小;添加剂的分子量越大、结构越复杂,越不容易发生迁移。     

不同材质食品接触材料及制品中PAEs合规情况调查及评价

目的 了解不同材质食品接触材料及制品中邻苯二甲酸酯类物质(Phthalate Esters,PAEs)的含量及分布情况,为食品接触材料及制品中邻苯二甲酸酯安全合规管理提供科学依据。方法 采用GC/MS对来自不同省市的781批不同材质食品接触材料测定其PAEs含量,从PAEs检出情况、量值分布、材质分布等维度对食品接触材料的PAEs安全合规情况进行了分析,并给出相关管控建议。结果 研究中测试的781批食品接触材料样品中,PAEs的总体检出率为12.8%(检出限为0.3 mg/kg),共检出6种PAEs。其中,邻苯二甲酸二(2–乙基)己酯(DEHP)检出率最高,为10.5%,其次为邻苯二甲酸二正丁酯(DBP)和邻苯二甲酸二异丁酯(DIBP),检出率分别为2.9%和1.7%。邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异壬酯(DINP)和邻苯二甲酸二环己酯(DCHP)检出率均低于0.5%。从检出量值来看,86.7%的检出数据小于10 mg/kg。不同材质食品接触材料中,橡胶制品的PAEs检出率最高,为50.0%,且检出物质多达5种;塑料制品的检出率为14.5%,仅3批PVC塑料中DEHP和1批橡胶制品中DINP检出数据大于100 mg/kg。结论 邻苯二甲酸酯在食品接触材料及制品中整体检出率较高,但检出数值高的占比较低,在橡胶和PVC塑料制品中检出率和检出数值相对较高,因此应高度关注其迁移风险。     

欧盟指令限制的与食品接触塑料中邻苯二甲酸酯类增塑剂迁移量的测定

建立了欧盟2007/19/EC指令中限制的对与食品接触的塑料材料中七种邻苯二甲酸酯迁移量的检测方法。样品采用食品模拟物浸泡后,取浸泡液用正乙烷进行液-液萃取,气相色谱仪/质谱联用仪（GC/MS）采用选择离子方式（SIM）检测,内标法定量。DBP、BBP、DEHP、nDnOP、DIDP、DINP、DAP检出限各为0.20...     

食品包装用PVC瓶盖垫片中增塑剂DEHP的迁移研究

为了解PVC垫片接触各类食品的安全性,采用气相色谱-质谱联用法研究了PVC垫片中DEHP在乙醇和正己烷中的迁移行为及其影响因素。实验结果表明:随着时间的延长,DEHP的迁出量逐渐增加;PVC垫片厚度越小,DEHP越容易迁出;与乙醇相比,DEHP更容易向正己烷中迁移,PVC垫片应避免接触脂肪类食品。     

食品接触材料中橄榄油总迁移量的风险分析

抽取8种材质273批食品接触材料及制品,对其进行适宜性判定、水分敏感性确认以及橄榄油总迁移量测试,分析不同材质食品接触材料的检出风险。结果表明,在适宜性判定方面,PVC材质适宜性判定不通过率为100%;PE、PET、氯乙烯-偏氯乙烯共聚树脂和纸铝塑盖膜材质的适宜性判定全部通过;TPE、PP及金属涂层材质则由于添加剂的干扰出现适宜性判定部分不通过。在水分敏感性方面,PET和纸铝塑盖膜试样均为水分敏感性试样,需要进行水分含量调节的概率为100%;TPE材质因添加剂、暴露时间等因素不同,需要进行水分含量调节的概率为48%;其他几种材质不需要进行水分含量调节。在迁移试验检出方面,TPE、PP和纸铝塑盖膜材质的检出风险较高,分别为86%, 58%, 50%;PE、PET、金属涂层材质检出率为7%, 9%, 9%,有一定的检出率,但是总体迁移风险不高;氯乙烯-偏氯乙烯共聚树脂材质加校正因子后符合限量要求。在迁移试验前,应优先做适宜性判定、水分敏感性确认及调节,确保测试结果的准确性与有效性,为食品接触材料及制品的安全管理和质量控制提供数据支持。     

油墨溶剂在食品软包装中的残留及迁移规律

目的研究油墨溶剂在食品软包装材料中的残留及迁移行为,为食品包装生产企业提供安全风险控制方面的参考。方法采用顶空气相色谱-质谱联用(HS-GC-MS)技术,对印刷油墨的挥发性溶剂在食品软包装中的残留进行定性定量分析,以检出率较高的苯类溶剂甲苯、酯类溶剂乙酸丁酯和酮类溶剂丁酮为迁移研究对象,分别以PE,PP,PET/CPP,PET/PE,OPP/CPP,PET/PA/CPP为包装材料,研究油墨溶剂在水性食品模拟液(蒸馏水)、酸性食品模拟液(体积分数为3%的乙酸)、醇性食品模拟液(体积分数为10%的乙醇)和脂肪性模拟液(正己烷)中的迁移残留行为。结果研究表明,印刷后的食品软包装材料中大部分都有苯类、酯类和酮类等有机挥发物的残留,残留溶剂在食品模拟液中迁移量的大小依次为正己烷乙醇(体积分数为10%)乙酸(体积分数为3%)蒸馏水,而且对于不同的包装材料迁移量的大小也不同。结论油墨溶剂在食品软包装材料上的残留和迁移行为,主要与环境温度、食品性质以及包装材料的性能有关。     

食品接触用纸制品中3-氯-1,2-丙二醇特定迁移量的测定

本文建立了食品接触用纸制品中3-氯-1,2-丙二醇在4%乙酸、10%乙醇和异辛烷3种食品模拟物中特定迁移的测定方法。采用食品模拟物浸泡,正己烷萃取,再经七氟丁酰基咪唑衍生,用气相色谱质谱法分析。在所选择的试验条件下,方法的线性良好,检出限低,测试样品的精密度和回收率也符合要求。     

PE淋膜纸中UV墨光引发剂向食品模拟物的迁移行为

研究聚乙烯(PE)淋膜纸4015、4025纸中紫外光(UV)固化墨光引发剂1-羟基环己基苯基甲酮(184)和2,2-二甲氧基-苯基甲酮(651)通过PE淋膜层向不同温度20℃、40℃和60℃、不同食品模拟物10%乙醇、95%乙醇和异辛烷中的迁移行为。探讨温度、迁移物分子结构、食品模拟物的溶胀、PE淋膜量对纸塑复合包装材料纸中具有不同分子结构的污染物通过不同厚度聚合物涂层向食品模拟物迁移的影响,从微观角度解释其影响因素。     

HDPE膜中Irgafos168在脂肪食品模拟物中的迁移试验研究

用反相高效液相色谱分析测定了不同温度下,正己烷、异辛烷和95%乙醇作为脂肪食品模拟物时,HDPE膜中Irgafos168的迁移量.探讨了温度和模拟物的选择对其迁移行为的影响.结果表明:用正己烷和异辛烷作为脂肪食品模拟物时,可以大大缩短迁移试验时间.温度加速了Irgafos168向脂肪食品模拟物的迁移,同时也影响其在包装材料与脂肪食品模拟物中的分配.     

中国和欧盟酸性食品模拟物对食品接触材料迁移量的差异性分析

目的 对中国和欧盟分别规定的不同酸性食品模拟物进行差异分析,并对2种不同酸性食品模拟物的迁移试验结果差异进行考察。方法 选取4类典型的酸性食品(共123种)进行pH测试,分别以3%(质量分数)的乙酸和4%(体积分数)的乙酸为食品模拟物对食品接触材料及制品进行迁移试验,并测试样品的总迁移量、甲醛迁移量、三聚氰胺迁移量、双酚A迁移量和重金属(锑)迁移量,比较样品在2种不同酸性食品模拟物中的迁移量差异。结果 pH测试结果表明,中国生产的4类酸性食品的pH范围为2.3~5.1,国外生产的4类酸性食品的pH范围为2.49~4.88,pH<5对4类酸性食品的pH覆盖率均大于或等于pH<4.5。迁移结果表明,在大多数情况下,食品接触材料在4%(体积分数)的乙酸中的迁移量,无论是总迁移量还是特定迁移量都大于或等于在3%(质量分数)的乙酸中的迁移量,食品接触材料在3%(质量分数)的乙酸中的迁移量高于在体积分数4%的乙酸的情况极少。结论 根据研究结果,中国采用pH<5定义酸性食品符合中国人的餐饮习惯,酸性食品覆盖性更广,更具合理性。迁移量测试结果表明,4%(体积分数)的乙酸是比3%(质量分数)的乙酸更为严苛的食品模拟物,因此对于国外出口中国的食品接触材料,即使已经按照欧盟标准采用3%(质量分数)的乙酸进行了迁移量测试,在进口到国内时还应用4%(体积分数)的乙酸按照中国相关标准再次进行迁移量测试,以满足中国标准的相关要求。     

Suitability of alternative fatty food simulants to study the effect of thermal and microwave heating on overall migration of plastic packaging

The suitability of alternative fatty food simulants on overall migration determination under thermal treatment and microwave heating were analysed for different plastic materials commonly used for packs subjected to thermal treatment or microwave heating. Elevated temperature and microwave heating increased overall migration. The results demonstrated that polymer–simulant affinity plays a large role in determining the suitability of the alternative simulant. For PA/PE, ethanol 95% represented the best alternative fatty food simulant to reproduce overall migration with olive oil. PVC presented a high overall migration. Microwave heating increased migration up to 45 mg/dm². For PVC, isopropanol was able to reproduce olive oil even after microwave heating. For PP, none of the alternative fatty food simulants were able to reproduce overall migration with olive oil. PP presented high inert behaviour. Microwave heating did not produce a significant increase in overall migration; meanwhile, the time of exposure produced a more significant migration. Copyright © 2004 John Wiley & Sons, Ltd.     

Investigations on Overall Migration of Various Plastic Materials and Articles Used in Contact with Foodstuffs

The results of overall migration tests for a wide range of plastic packagings and other domestic and imported articles made of plastic intended to come into direct contact with foodstuffs are presented. In these tests the simulants specified in Directive 85/572/EEC as well as isooctane and 95% ethanol (so called alternative substances) have been used. Checking the overall migration into the four simulants specified in the above mentioned Directive it was found that the limit (equal to 10 mg/dm² according to Directive 90/128/EEC) was exceeded in a few, very specific, cases. Comparison between overall migration from some articles into sunflower oil and isooctane was also examined. The results indicate that though the use of isooctane as an alternative substance significantly simplifies the testing procedure, exceeding an overall migration limit into isooctane is not equivalent to exceeding the limit of migration into sunflower oil. In such cases only migration into typical fatty food simulants can have a deciding meaning. © 1997 John Wiley & Sons, Ltd.     

A systematic study on the stability of UV ink photoinitiators in food simulants using GC

Several studies have been published on the stability of plastic monomers and additives in food simulants. However, there are practically no published results about the stability of ink components in food simulants. In this work, the stability of two ultraviolet (UV) ink photoinitiators (PIs) in one aqueous and in two substitute fat food simulants was studied under various time–temperature conditions. Furthermore, the addition of the stabilizing agent hydroquinone monomethyl ester (HQMME) in the same conditions was considered as a comparative experiment. The PIs tested were 1‐hydroxycyclohexyl‐1‐phenyl ketone (Irgacure‐184) and benzyldimethyl ketal (Irgacure‐651). The various test conditions included exposure of 10 days to temperatures of 20, 40 and 60°C for 10% ethanol and 95% ethanol simulants, and exposure of 2 days to temperatures of 20, 40 and 60°C for isooctane. Following exposure to these conditions, the additive samples were analysed. The extracts of samples exposed to various temperature conditions as well as unexposed spiked controls and blanks were analysed by gas chromatography (GC) on a non‐polar (5%‐phenyl)‐methylpolysiloxane capillary column. The results showed that the protective effect of HQMME was not obvious in all test conditions under dark conditions. The Irgacure‐184 was quite stable under all test conditions whether the stabilizing agent was added or not. Irgacure‐651 was stable almost under all test conditions, except in 10% ethanol at 60°C. The mass spectrum of decomposed product of Irgacure‐651 was detected by GC‐MS (Mass Spectrum), and the structure of the decomposed product was obtained by mass spectrographic analysis. The method of detection and disposal is also applicable for UV ink PI migration testing from several different paper or paperboard‐plastic coating layer materials into the food simulants used in the study. Copyright © 2008 John Wiley & Sons, Ltd. 2008     

食品接触用多层复合包装中迁移物质的非靶向筛查和风险评价

目的 以食品接触用纸/铝/塑复合包装为研究对象,结合应用非靶向高通量筛查技术和安全风险评价方法,全面研究这类多层复合包装在接触食品过程中的迁移风险。方法 采用顶空气相色谱-串联质谱、气相色谱-四极杆飞行时间质谱和液相色谱-四级杆飞行时间质谱全面筛查食品接触用纸/铝/塑复合包装在不同迁移条件下的挥发性、半挥发性和非挥发性迁移物质,基于商业数据库、实验室自建库及行业信息解析物质化学结构及可能来源,利用内标半定量迁移水平,结合国内外食品接触材料法规和安全风险评估方法进行符合性评价及风险评价。结果 20批纸/铝/塑复合食品包装在体积分数为4%的乙酸模拟物中未发现迁移风险,在体积分数为95%的乙醇模拟物中共计检出35种物质,可能源于溶剂、抗氧剂、爽滑剂、低聚物、抗氧剂氧化/降解产物等物质。其中,33种物质经法规评估及毒理学评估,显示风险较低;其余2类聚烯烃低聚物因结构难以确定、缺乏毒理学研究建议持续关注毒理学研究进展及国内外法律法规动态。结论 通过结合应用非靶向高通量筛查技术和安全风险评估方法研究表明,在通常的使用条件下,纸/铝/塑多层复合包装用于盛装果汁等水性食品时不存在安全风险,但接触高乙醇含量或油脂类食品时建议关注聚烯烃类低聚物的迁移安全性。     

Electrospray Ionization‐Mass Spectrometry Analysis Reveals Migration of Cyclic Lactide Oligomers from Polylactide Packaging in Contact with Ethanolic Food Simulant

Electrospray ionization‐mass spectrometry analysis revealed rapid migration of cyclic oligomers from polylactide (PLA) packaging when stored in contact with 96% ethanol. The mass losses in contact with water, 3% acetic acid, 10% ethanol and isooctane were 3 to 5 times smaller and no migration of cyclic oligomers was observed. The presence of cyclic oligomers in the original PLA films and their solubility in ethanol, thus, explains the rapid mass loss for PLA in contact with ethanolic food simulant. On prolonged ageing no further mass loss was observed in 96% ethanol, whereas mass loss in aqueous food simulants increased because of hydrolysis of PLA matrix or the cyclic oligomers to water‐soluble linear products. The mass losses were generally somewhat smaller for the stereocomplex material compared with the poly‐l ‐lactide materials. Similar trend was observed for solvent uptakes, which is easily explained by the higher degree of crystallinity and stronger secondary interactions in the stereocomplex material. The use of ethanol as a fatty food simulant for PLA materials could, thus, lead to overestimation of the overall migration values. Copyright © 2012 John Wiley & Sons, Ltd.     

Migration of Cyclic Monomer and Oligomers from Polyamide 6 and 66 Food Contact Materials into Food and Food Simulants: Direct Food Contact

Cyclic monomer and oligomers are the major migrating substances from polyamide (PA) food contact materials. An increase of caprolactam (+44%) and cyclic oligomer content (+27%, incl. caprolactam) in PA6 was observed by thermal treatment, here by extrusion of a PA6 film from a granulate. Migration experiments with a PA6 and a PA66 packaging film were carried out into food simulants according to directives 85/572/EEC and 82/711/EEC. Contact conditions (2 h/100°C) were chosen for a heat treatment of the food in the packaging, in this case production of scalded sausage. Aqueous and ethanolic food simulants clearly revealed to be the worst case for migration of cyclic PA6 and PA66 monomer and oligomers. Migration of cyclic oligomers into oil was one order of magnitude lower. No migration could be observed into isooctane (<8 µg dm^?2). The substitutes for oil, 95% ethanol and isooctane, were inapplicable for simulating migration of cyclic oligomers into oil. Caprolactam showed different migration behaviour compared with cyclic oligomers, migrating into oil and water to the same extent depending on contact conditions. Fifty percent of the extractable caprolactam migrated from a PA6 sausage casing into scalded sausage (4.2 mg kg^?1), residual 41% apparently were extracted by the boiling medium or during pretreatment (soaking) of the casing. Potential migration of caprolactam and cyclic oligomers from a PA6 tea bag was found to be 18% of the specific migration limit for caprolactam and 36% of the overall migration limit. Copyright © 2014 John Wiley & Sons, Ltd.     

食品接触用银制品中8种重金属元素迁移量研究

目的考察重金属含量、食品模拟物、迁移温度和迁移时间这4个因素对食品接触用银制品中Ag,As,Pb,Cd,Cr,Ni,Sb,Zn迁移量的影响。方法试样按照充填浸泡和全浸泡的方法分别浸泡于乙酸(体积分数为4%)、乙醇(体积分数为10%,50%,95%)食品模拟物中,浸泡迁移完成后提取10 mL浸泡液用ICP-AES测定。结果8种重金属元素中Ag,Cr,Ni,Zn被检出,重金属元素迁移量随着该元素在食品接触用银制品中含量的增高而增高;乙醇(体积分数为10%,50%,95%)食品模拟物中重金属元素迁移量较低,体积分数为4%的乙酸食品模拟物中重金属元素迁移量明显增高;8种金属元素的迁移量随着浸泡温度的升高和浸泡时间的延长而逐渐增高。结论食品接触用银制品中8种重金属元素的迁移量与该元素在银制品中的含量有关,食品接触用银制品在接触酸性食品时存在较大质量安全隐患,很容易造成食品中Ag,Cr含量超标。为提高银制餐具的贸易销售提供了理论支持,为监管部门及时发现产品潜在安全风险提出了合理建议,也为食品接触用银制品中重金属元素迁移量的限量指标提供了数据参考。