纸质包装材料中邻苯二甲酸酯类物质向Tenax和奶粉的迁移

采用气相质谱联用对100、70与50℃条件下10种邻苯二甲酸酯类物质从微波纸和牛皮纸向脂肪类模拟物Tenax和奶粉中的迁移行为进行了研究。以温度、分子结构、纸张特性等为主要考虑因素,探究了邻苯二甲酸酯类物质的迁移行为。结果表明,邻苯二甲酸酯类物质的迁移行为受温度、时间、纸张特性、分子量等因素影响,一般随着温度的升高、纸张克重及厚度减小、分子量的降低,最大迁移率越高,但迁移率也受到分子结构及迁移底物的影响。     

超高压液相色谱法测定食品接触材料印刷油墨中光引发剂

目的 建立超高压液相色谱-二极管阵列检测器(UPLC-DAD)快速测定食品接触材料表面印刷油墨中光引发剂的分析方法。方法 采用65%和正己烷作为食品模拟物模拟含酒精和脂肪食品, 分别在5 ℃和40 ℃的温度下进行240 h的迁移试验。迁移后的模拟液经浓缩、净化、重新溶解并过滤后直接进样分析。结果 线性范围为0.1~500.0 μg/L, 检出限为0.005 μg/dm2, 空白样品的加标回收率为79.8%~92.3%。采用UPLC-DAD对30余种食品接触材料中光引发剂种类和含量进行了测定。ITX和EHDAB在食品接触材料中一般协同出现, 其迁移水平分别为0.11 μg/dm2和0.092?0.370 μg/dm2。结论 超高压液相色谱-二极管阵列检测器(UPLC-DAD)可以用于快速测定食品接触材料表面印刷油墨中光引发剂。     

食品包装纸中模拟污染物迁移行为的研究

纸和纸板广泛用作食品包装材料,主要用于包装一次性产品。但是食品包装纸中含有一些污染物会迁移到食品中从而威协到消费者的安全。食品包装纸中污染物对食品的污染程度是由迁移到食品中的能力决定的。论文主要研究白卡纸中模拟污染物邻二甲苯、苯乙酮、正十二烷、萘、二苯醚、二苯甲酮、邻苯二甲酸二异丁酯、硬酯酸甲酯在不同温度下向干性食品全脂奶粉和Tenax的迁移规律。研究发现,模型污染物的化学性质不同,向干性食品中的迁移能力不同。食品或食品模拟物的性质也会影响迁移能力。研究还表明,接触时间以及温度对模拟污染物向食品中的迁移都具有很大的影响。     

UV油墨光引发剂EDB在食品软包装中的迁移分析

为研究UV油墨光引发剂4-二甲氨基苯甲酸乙酯(EDB)在食品软包装中的迁移行为,制作了实际印刷、直接污染和蹭脏污染三种包装试样,分别以3%(w/v)乙酸、10%(v/v)乙醇和95%(v/v)乙醇作为酸性、酒精类和脂类食品模拟液,研究了EDB的迁移和残留行为。结果表明,光引发剂EDB在三种包装试样中都发生迁移。在三种食品模拟液中,EDB向95%乙醇中的迁移量最大,且初始迁移速率最快,说明EDB更容易向脂类模拟物迁移。温度越高,迁移量越大,达到平衡的时间越短。     

微波条件下纸包装油墨中增塑剂向食品（模拟物）的迁移

研究纸张印刷油墨中4 种增塑剂（3 种邻苯二甲酸酯类增塑剂和近年流行的环保增塑剂乙酰基柠檬酸三丁酯）向食品模拟物Tenax和奶粉的迁移,考察其在110、250、440、600、900 W微波功率下的迁移行为,探讨迁移影响因素,并与常规条件下的迁移行为做比较。结果显示在一定条件下微波功率越高,迁移量越大;且迁移行为受增塑剂的分子质量、极性等性质的影响;常规条件下的迁移影响因素也适用于微波条件。     

食品包装纸中的饱和烃矿物油向食品模拟物Tenax的迁移和安全评估

研究食品包装纸中饱和烃矿物油(MOSH)向食品模拟物Tenax的迁移,考虑了不同类型包装纸在不同温度下(25℃、40℃、100℃)的迁移行为,并采用毒理学关注阈值(TTC)的方法对MOSH进行安全评估。结果表明:温度一定时,厚度和克重是影响食品包装纸中MOSH迁移的重要因素,厚度和克重越小,MOSH的迁移率越大;在一定条件下,温度越高,MOSH达到迁移平衡的时间越短(100℃,100 min;25℃,8 d),迁移率越大(100℃,24.81%;25℃,7.82%)。所测定的包装纸中MOSH达到迁移平衡时的迁移量,都明显超过了JECFA规定的特定迁移量0.6 mg/kg,容易发生迁移的MOSH主要集中在C16~C18和C23~C26,均属于容易在人体内蓄积的中低粘度矿物油。TTC评估结果表明:主要发生迁移的MOSH烃类经Cramer分类均属于Class I,从四种食品包装纸中迁移到Tenax的MOSH,估计每日摄入量(EDI)均明显高于对应的TTC阈值(1.8 mg/person·day),需要引起关注。     

陶瓷食品包装材料中铅、镉向真实食品的迁移研究

陶瓷食品包装容器中的有害重金属铅、镉向食品的迁移会造成食品污染进而危害消费者身体健康.本文通过制备含有铅、镉这两种重金属元素的陶瓷样品,使之分别在20℃和40℃的条件下与白酒、黄酒、醋和酸豆角汁这四种真实食品接触一定时间来研究这两种重金属的迁移行为.结果表明:铅、镉迁移量随着温度的升高而增加,并且迁移速率也与温度成正比;铅、镉的迁移量受食品的pH影响,pH越低,迁移量越高;铅的迁移量还与酒精度成反比,酒精度越高,铅的迁移量越少.     

食品用纸杯中光引发剂特定迁移量的气相色谱- 串联质谱测定方法

目的建立11种光引发剂类化合物食品用纸杯特定迁移量的气相色谱-串联质谱(gas chromatographytandem mass spectrometry,GC-MS/MS)检测方法。方法食品模拟物中的光引发剂类化合物经反相固相萃取柱富集净化后,采用中等级性的DM-17MS气相色谱柱进行分离;采用三重四极质谱的多反应监测模式(multiple reaction monitoring,MRM)对化合物进行定量测定。结果本方法可在17 min内完成11种目标化合物的色谱分离。11种光引发剂在低、中、高3个添加水平的回收率在65.0%~119.8%范围内,相对标准偏差为1.2%~10.6%(n=6),方法检出限为1~7μg/L,定量限为2~20μg/L。结论该方法灵敏度高,定量准确,适用于食品模拟物中光引发剂类物质特定迁移量的测定。     

食品接触用不锈钢材料中铬元素迁移规律

为探究不同食品加工条件对食品接触用304、316不锈钢中铬(Cr)元素迁移规律的影响,通过全浸泡迁移实验结合电感耦合等离子体质谱检测法(inductively coupled plasma-mass spectrometry, ICP-MS)测得在不同温度、高温煮沸、高压蒸汽灭菌等生产条件下,不锈钢中Cr向体积分数为4%的乙酸食品模拟液中的迁移量随时间的变化情况,分析Cr迁移与生产条件关系。结果表明,不同生产条件下,不锈钢主要组成元素Cr迁移量随接触时间延长及加工温度的升高而增大。20、70℃温度条件下长时间迁移Cr元素平均迁移速率为40℃时的1/3与4倍;煮沸、高压蒸汽灭菌短时迁移时Cr平均迁移速率较40℃分别提高约为4和9倍。温度越高,不锈钢中Cr迁移量越大,尤其是煮沸、高压蒸汽灭菌等特殊工况对重金属向食品模拟物中的迁移具有明显的促进作用。对迁移数据进行拟合发现,Cr迁移行为符合Fick定律,其扩散系数与温度相依性可采用阿伦尼乌斯定律来表示。     

纸包装油墨中增塑剂向奶粉的迁移

纸包装油墨中含有有毒有害物质并可通过包装材料迁移进入内装食品从而危害人体健康。模拟实际印刷条件制作真实油墨迁移单元,研究纸张胶印油墨中4种主要增塑剂（3种邻苯二甲酸酯类增塑剂和近年流行的环保增塑剂乙酰基柠檬酸三丁酯）向奶粉的迁移,考察其在100、70、50、25 ℃的迁移行为,探讨增塑剂的性质及其在纸张中的分布等因素对迁移行为的影响。结果表明：4种增塑剂的最大迁移率在6.7%～67.8%之间。纸包装油墨中增塑剂的迁移防护性能还有待提高。     

高温下白卡纸中二苯甲酮和1-羟基环己基苯基甲酮向食品模拟物质的迁移

研究了在70℃和90℃下,采用直接浸泡法使白卡纸中的固化剂二苯甲酮(BP)和1-羟基环己基苯基甲酮(HCH)向水、3%乙酸、15%乙醇、50%乙醇、95%乙醇等食品模拟物质迁移,采用高效液相色谱仪(HPLC)分别检测迁移后模拟物质中的迁移量。结果表明两种固化剂在0.64~40mg/L的质量浓度范围内呈良好线性,相关系数不小于0.9995。温度越高,迁移时间越长,迁移量也越大;随着乙醇浓度的增高,BP、HCH的迁移量也增加;对于3%乙酸,BP和HCH迁移率最小。     

快餐包装纸中矿物油向固体食品模拟物的迁移

研究从市场上收集到的24 种快餐包装纸中的矿物油向固体食品模拟物Tenax的迁移规律。在多个不同的迁移条件（40 ℃/0.5、1、2、3 h,40 ℃/10 d和70 ℃/2 h）,探究矿物油的迁移行为及其影响因素,以评价其安全性。选择正己烷-乙醇（1∶1,V/V）混合溶液对Tenax进行过夜萃取,采用质量分数0.3%硝酸银固相萃取柱对饱和烃矿物油（mineral oil saturated hydrocarbons,MOSH）和芳香烃矿物油（mineral oil aromatic hydrocarbons,MOAH）进行分离纯化,最后用气相色谱-氢火焰离子化检测法和气相色谱-质谱法分别进行定量和定性分析。结果表明：随着温度的升高,多种快餐包装纸中矿物油向Tenax的迁移量也随之增加。涂蜡纸中MOSH迁移量均有所检出,其数值为110.49～615.40 mg/kg,而MOAH部分均未检出,这可能是因为涂蜡纸表面涂覆的石蜡层属于MOSH类,导致其MOSH部分的迁移量较高。网购餐盘纸和常规餐盘纸中MOSH迁移量约为其特定限量值（0.6 mg/kg）的10～400 倍,MOAH的迁移量约为其特定限量值（0.5 mg/kg）的10～70 倍,而使用优质胶印油墨的原生纤维餐盘纸均未超过其限量值。最后,通过对印有胶印油墨的原生纤维餐盘纸中矿物油进行溯源分析,发现经过迁移的矿物油一部分可能来源于其所用油墨,其他来源可能来自于回收纤维、黏合剂、添加剂和加工助剂等。     

Migration of photoinitiators from cardboard into dry food: evaluation of Tenax® as a food simulant

Photoinitiators are widely used to cure ink on packaging materials used in food applications such as cardboards for the packaging of dry foods. Conventional migration testing for long-term storage at ambient temperature with Tenax^® was applied to paperboard for the following photoinitiators: benzophenone (BP), 4,4?-bis(diethylamino)benzophenone (DEAB), 2-chloro-9H-thioxanthen-9-one (CTX), 1-chloro-4-propoxy-9H-thioxanthen-9-one (CPTX), 4-(dimethylamino)benzophenone (DMBP), 2-ethylanthraquinone (EA), 2-ethylhexyl-4-dimethylaminobenzoate (EDB), ethyl-4-dimethylaminobenzoate (EDMAB), 4-hydroxybenzophenone (4-HBP), 2-hydroxy-4-methoxybenzophenone (HMBP), 2-hydroxy-4?-(2-hydroxyethoxy)-2-methylpropiophenone (HMMP), 2-isopropyl-9H-thioxanthen-9-one (ITX), 4-methylbenzophenone (MBP) and Michler’s ketone (MK). Test conditions (10 days at 60°C) were according to Regulation (EU) No. 10/2011 and showed different migration patterns for the different photoinitiators. The results were compared with the migration in cereals after a storage of 6 months at room temperature. The simulation with Tenax at 60°C overestimated actual migration in cereals up to a maximum of 92%. In addition, the effect of a lower contact temperature and the impact of the Tenax pore size were investigated. Analogous simulation performed with rice instead of Tenax resulted in insufficiently low migration rates, showing Tenax is a much stronger adsorbent than rice and cereals.     

火麻仁青稞膨化饼干配方及关键工艺优化

以火麻仁、青稞粉为主要原料,利用火麻仁中的不饱和脂肪酸替代饼干加工中油脂的添加,研发出新型休闲食品-火麻仁青稞膨化饼干。结果表明:通过L8(27)正交试验获得以100 g中筋粉为基准的原辅料最佳配比为青稞粉45%、谷朊粉1%、可可粉3%、魔芋精粉10%、蔗糖10%、纯净水50%、火麻仁浆35%;最佳工艺参数为压面厚度2.50 mm、空气膨化温度182℃、空气膨化时间8 min,此条件下成品综合品质最佳。     

Kinetic migration of isothiazolinone biocides from paper packaging to Tenax and Porapak

Migration investigations were carried out on paper packaging materials in contact with solid food simulants. The aim was to investigate the migration behaviour of a series of isothiazolinone biocides (2-methyl-3-isothiazolinone (MI), 1,2-benzisothiazolinone (BIT) and 2-octyl-3-isothiazolinone (OIT)) as potential contaminants in paper materials, at varying temperatures and migration times, for the food simulants Tenax and Porapak. Based on the migration results, Tenax was found to be a good food simulant, and was more suitable than Porapak at high temperature. Petri dishes were found to be suitable for use as migration cells when the compounds to be evaluated were non-volatile. The amount of migration gradually increased with time and increasing temperature, finally reaching a steady value. When the temperature was higher than the boiling point of OIT, the migration rate decreased because of volatilization. The maximum migration rates were 3.4% for MI, 2.2% for BIT and 10.6% for OIT at high temperature (≥100 °C). Two kinds of paper packaging for food were tested with the method that was developed. OIT in the papers migrated into the food simulants but the amount that migrated was less than 0.14 μg kg(-1).     

Investigation of migration from paper and board into food-development of methods for rapid testing

A range of paper and board materials including carton board, corrugated board, napkins and paper towels intended for contact with food have been solvent extracted and substances present at the highest levels identified and quantified by GC/MS. Dibutyl phthalate, and diisopropylnaphthalene (DIPN) were selected to study migration to food and potential food simulants with the aim of developing a simple quick test that will give an equivalent or higher result. Tenax was found to be a suitable food simulant for dry foods and dry 'fatty foods' such as pastry and cake and was also found to be a suitable simulant for pizza base tested at higher temperatures for short contact times. The percentage migration values from corrugated and carton boards were generally in the range 15-40%, with the highest percentage being 49% for rice using conditions representing ambient storage. Quick tests were developed using Tenax under accelerated conditions of 4h at 80°C to cover room temperature storage with dry foods and fatty dry foods. These tests are suitable for compliance testing of paperboard samples if migration limits are applied in future legislation. Migration from tissues, napkins and paper towels was found to be at very low or not detectable levels, even when the levels of DIPN and DBP were significant. It is strongly suspected that this finding is due to a combination of short contact time, low grammage and the fact that the tissues absorb fat and moisture from foods, thus minimizing extraction from the paper. In all cases, the results from migration experiments into food and Tenax indicate that for the substances found at highest concentrations in the paper, currently accepted safety limits were not exceeded where they exist in EU legislation or in working documents applying to plastics.     

Use of Tenax® films to demonstrate the migration of chemical contaminants from cardboard into dry food

ABSTRACT

Contaminants in food packaging are a challenge of our time since the packaging material itself has been found to represent a source of food contamination through the migration of substances from it. Before first use, packaging materials destined for the packaging of dry foods can be evaluated by performing migration experiments with the simulant for dry foods, Tenax®. This simulant is commercially available as a powder that is more difficult to handle during the migration experiments. This paper reports the development of a Tenax film. The film can be applied to the cardboard surface to conduct the migration test. After the migration is completed, the film can be easily extracted to determine the concentration of the contaminants in the film. Finally, the performance of the Tenax film was compared with the conventional Tenax powder for the evaluation of 15 model migrants.     

免疫牛初乳与双歧杆菌复合微胶囊的研制

以双歧杆菌发酵免疫牛初乳,然后采用真空冷冻干燥技术研制成冻干粉,并以冻干粉为芯材、以肠溶材料欧巴代为壁材、以保护剂为润湿剂,采用空气悬浮微胶囊化的方法制成免疫与微生态双活性肠溶制剂。通过正交试验确定空气悬浮造粒机的最佳工艺参数为进风量200m3/h、进气温度45℃、排气温度36℃、物料温度37℃、喷浆速率6r/min。得到的微胶囊产品为浅绿色圆形颗粒状、不粘连、流动性好、粒径大小基本均匀。     

Migration of photoinitiators from paper to fatty food simulants: experimental studies and model application

The migration of five different photoinitiators from kraft paper to two fatty food simulants, Tenax^® and 95% ethanol, was investigated under different conditions. The effects of temperature and storage time, as well as the physicochemical properties of the photoinitiators on migration, were discussed. Mathematical models based on Fick’s second law generated from two cases, single- and two-side contacts, were applied to predict the migration behaviour from the paper to the food simulants. The partition coefficients estimated from the model decreased with temperature. The diffusion coefficients of the selected photoinitiators from the paper ranged from 1.55 × 10^–10 to 7.54 × 10^–9 cm² s^?1 for Tenax and from 2.79 × 10^–9 to 8.03 × 10^–8 cm² s^?1 for 95% ethanol. The results indicate that the applied model can predict the migration of photoinitiators in the initial short period before equilibrium, and the migration from paper to Tenax through a single-side contact demonstrated an especially high concordance.